S News Continuously updated synthesis method about 72291-30-6

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 72291-30-6, name is Methyl 2-cyano-2-methylpropanoate, A new synthetic method of this compound is introduced below., Safety of Methyl 2-cyano-2-methylpropanoate

At -10C, hydrogen chloride gas was bubbled into an ethanol (50 ml) solution of 8.00 g of the mixture of cyano-dimethylacetic acid ethyl ester and cyano-dimethylacetic acid methyl ester (I-69), while stirring for 6 hours. After concentration of the reaction solution, ether was added to the thus obtained residue and stirred for 30 minutes, and the precipitated crystals were collected by filtration and dried to obtain 8.2 g of the title compound as a colorless solid. This was directly used in the subsequent reaction.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; DAIICHI PHARMACEUTICAL CO., LTD.; EP1717238; (2006); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Research on new synthetic routes about Methyl 2-cyano-2-methylpropanoate

The synthetic route of 72291-30-6 has been constantly updated, and we look forward to future research findings.

Reference of 72291-30-6, A common heterocyclic compound, 72291-30-6, name is Methyl 2-cyano-2-methylpropanoate, molecular formula is C6H9NO2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

The experiment examples are carried out in a 1 l reactor (10×2000 mm), equipped with feed pumps for solvent, ammonia and nitrile ester, charged with 250 ml of steel rings in the lower and upper reactor section, and centrally with 500 ml of tablets (5×3 mm) of a hydrogenation catalyst of the following composition: 28% NiO, 28% CoO, 13% CuO and 31% ZrO2, in liquid phase mode. The reduction procedure of the catalyst is as follows: the reactor is heated to 180 C. at a hydrogen feed of 50 l/h within 5 hours, then kept at 180 C. with 50 l/h of hydrogen for 20 hours, cooled under hydrogen and purged with MeOH, before ammonia and reactant and also solvent are fed in. The steel rings in the lower part of the reactor serve as the delay time zone for the amidation. 11 equivalents of hydrogen are fed in per nitrile used. The delay time is thus approx. 10 minutes. Example 10250 g/h of tetrahydrofuran (THF) and methyl 2-cyano-2,2-dimethylacetate as the nitrile ester (in a weight ratio of 70:30) and 205 g of ammonia (20 equivalents of ammonia based on nitrite ester) are conducted through the reactor at 200 bar and 100 C. The volume space velocity is 0.15 kg/l*h. The effluent analysis shows (calculated without solvent) 33.083% aminopivalinamide, 65.68% methyl aminopivalate and 0.49% others. The delay time is approx. 27 minutes.

The synthetic route of 72291-30-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BASF SE; US2008/306299; (2008); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Analyzing the synthesis route of C6H9NO2

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Methyl 2-cyano-2-methylpropanoate, other downstream synthetic routes, hurry up and to see.

Electric Literature of 72291-30-6, The chemical industry reduces the impact on the environment during synthesis 72291-30-6, name is Methyl 2-cyano-2-methylpropanoate, I believe this compound will play a more active role in future production and life.

A mixture of cyano-dimethyl-acetic acid methyl ester (5 g, 39.4 mmol), Boc anhydride (17.2 g, 78.7 mmol), and NiCl2 (0.51 g, 3.94 mmol) in MeOH (200 mL) was cooled in an ice bath. NaBH4 (10.4 g, 276 mmol) was slowly added over 1 h at 0C, and the resulting mixture was stirred at r.t. for 16 h. Diethylenetriamine (4.3 mL, 39.4 mmol) was then added, and the mixture was stirred for 30 min. The solvent was evaporated, and the residue was partitioned between EtOAc (200 mL) and saturated NaHCC>3 (400 mL). The aqueous layer was extracted with additional EtOAc, and the organic layers were combined, dried over MgSO/t, and concentrated. The crude product was purified by column chromatography (0-40% EtOAc/hexanes) to give 2.5 g of the title compound as a clear oil. H NMR (CDCI3, 200 MHz): 8ppm= 4.95 (br s, 1H), 3.69 (s, 3H), 3.24 (d, 2H, J= 6.6 Hz), 1.44 (s, 9H), 1.20 (s, 6H).

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, Methyl 2-cyano-2-methylpropanoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; FIBROGEN, INC.; HO, Wen-Bin; ZHAO, Hongda; DENG, Shaojiang; NG, Danny; WRIGHT, Lee R.; WU, Min; ZHOU, Xiaoti; AREND, Michael P.; FLIPPIN, Lee A.; WO2013/134660; (2013); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Discovery of C6H9NO2

The synthetic route of Methyl 2-cyano-2-methylpropanoate has been constantly updated, and we look forward to future research findings.

These common heterocyclic compound, 72291-30-6, name is Methyl 2-cyano-2-methylpropanoate, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Recommanded Product: Methyl 2-cyano-2-methylpropanoate

50L adding glass cauldron 25L methanol, add 2.20 kg potassium hydroxide (39.4mol), stirring then after cooling to room temperature, dropping 5.00kg2-cyano-2-methyl propane acid methyl ester (39.4mol), stirring reaction after dropping 2h; reaction the fluid turns on lathe dry, solid with a small amount of anhydrous ethanol after washing, 50 C drying, obtain 5.53kg2-cyano-2-methyl propane acid potassium, molar yield 93%.

The synthetic route of Methyl 2-cyano-2-methylpropanoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hefei Leaf Biotechnology Limited; Deng, Jin; Wang, Peng; Fu, Yao; Ding, Fan; Xu, Qiang; Xu, Hai; Yu, Sanxi; Ding, Feijiao; Wu, Jiangjiang; Huang, Ligang; Xu, Shengchun; (8 pag.)CN105541594; (2016); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Continuously updated synthesis method about 72291-30-6

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 72291-30-6, name is Methyl 2-cyano-2-methylpropanoate, A new synthetic method of this compound is introduced below., COA of Formula: C6H9NO2

At -10C, hydrogen chloride gas was bubbled into an ethanol (50 ml) solution of 8.00 g of the mixture of cyano-dimethylacetic acid ethyl ester and cyano-dimethylacetic acid methyl ester (I-69), while stirring for 6 hours. After concentration of the reaction solution, ether was added to the thus obtained residue and stirred for 30 minutes, and the precipitated crystals were collected by filtration and dried to obtain 8.2 g of the title compound as a colorless solid. This was directly used in the subsequent reaction.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; DAIICHI PHARMACEUTICAL CO., LTD.; EP1717238; (2006); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Simple exploration of Methyl 2-cyano-2-methylpropanoate

The synthetic route of 72291-30-6 has been constantly updated, and we look forward to future research findings.

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 72291-30-6, name is Methyl 2-cyano-2-methylpropanoate belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. category: nitriles-buliding-blocks

The experiment examples are carried out in a 1 l reactor (10×2000 mm), equipped with feed pumps for solvent, ammonia and nitrile ester, charged with 250 ml of steel rings in the lower and upper reactor section, and centrally with 500 ml of tablets (5×3 mm) of a hydrogenation catalyst of the following composition: 28% NiO, 28% CoO, 13% CuO and 31% ZrO2, in liquid phase mode. The reduction procedure of the catalyst is as follows: the reactor is heated to 180 C. at a hydrogen feed of 50 l/h within 5 hours, then kept at 180 C. with 50 l/h of hydrogen for 20 hours, cooled under hydrogen and purged with MeOH, before ammonia and reactant and also solvent are fed in. The steel rings in the lower part of the reactor serve as the delay time zone for the amidation. 11 equivalents of hydrogen are fed in per nitrile used. The delay time is thus approx. 10 minutes.Example 9503 g/h of MeOH and, as the nitrile ester, methyl 2-cyano-2,2-dimethylacetate (in a weight ratio of 1:1) and 670 g of ammonia (20 equivalents of ammonia based on nitrile ester) are conducted through the reactor at 200 bar and 100 C. The volume space velocity is 0.5 kg/l*h. The effluent analysis shows (calculated without solvent) 99.89% aminopivalinamide, 0.03% methyl aminopivalate and 0.08% others. The delay time is approx. 9.8 minutes.

The synthetic route of 72291-30-6 has been constantly updated, and we look forward to future research findings.

Introduction of a new synthetic route about 72291-30-6

The chemical industry reduces the impact on the environment during synthesis Methyl 2-cyano-2-methylpropanoate. I believe this compound will play a more active role in future production and life.

Synthetic Route of 72291-30-6, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 72291-30-6, name is Methyl 2-cyano-2-methylpropanoate, This compound has unique chemical properties. The synthetic route is as follows.

The reactant and the catalyst are initially charged in the autoclave and the contents are inertized by purging with nitrogen. Subsequently, 5 bar of hydrogen are injected. The desired amount of ammonia is metered in and then the autoclave is heated slowly with stirring to the reaction temperature (80 C.). This step takes an average of 90 min, i.e. the delay time of the reactant solution in contact with ammonia is approx. 90 min. On attainment of the reaction temperature, hydrogen is injected rapidly to the pressure specified in Table 1 below and consumed hydrogen is replaced by metering under pressure control over the experiment time until no further hydrogen absorption is recorded.The autoclave experiments are carried out in a 2.5 l autoclave with hollow-shaft disk stirrer (stirrer speed approx. 600 rpm), electrical heating and jacket air cooling, 2 baffles, sparging through the autoclave lid and introduction of the hydrogen via the hollow-shaft stirrer. The weights for Raney catalysts are corrected for 10% water moisture, i.e., in real terms, 10% more water-moist catalyst is weighed out than specified. Reaction effluents are analyzed via gas chromatography (GC) (conditions: 60 m DB1701; internal diameter 0.32 mm; film thickness 0.25 mum; detector: FID; temperature program: 80 C.?10 K/min?280 C., 40 min, split ratio 100:1, carrier gas helium) and the compositions are reported in % by weight.The reactor yield is determined by means of gas chromatography with internal standard (I.S.) (I.S. piperidine; the concentration thus obtained in the crude effluent is multiplied by the total mass of the crude effluent and the yield thus calculated is compared to the theoretical yield). The reactions are all carried out with methyl 2-cyano-2,2-dimethylacetate with a purity of >99.8%. The main product obtained is aminopivalinamide (3-amino-2,2-dimethylpropionamide). TABLE 1 Pressure/ % by weight ConcentrationNH3/ Purity Conversion Reactor Example bar Catalyst of catalyst Solvent % nitrile (crude, GC) % % yield % 1 200 Ra-Ni 10 NMP 30 20:1 98.7 100 not determined 2 65 Ra-Co 10 BuOH 40 7.7:1 98.8 100 94.0% 3 65 Ra-Ni 10 BuOH 40 7.7:1 98.2 99.7 90.6% 4 65 Ra-Ni 2.5 BuOH 40 3:1 93.7 99.7 84.9% 5 65 Ra0Co 2.5 BuOH 40 3:1 94.9 99.9 86.7 6 65 Ra-Co 5 MeOH 40 3:1 96.5 99.1 90.4 7 65 Ra-Co 5 MeOH 40 3:1 96.6 99.1 91.1 8 65 Ra-Co 5 BuOH 40 3:1 90.0 99.4 88.2 The examples show that very good selectivities of at least 90% are achievable with Raney nickel and Raney cobalt. The higher the amount of ammonia, the higher the catalyst concentration and the higher the hydrogen pressure, the better is the selectivity. In example 8, a metal determination is carried out, 430 ppm of Co are found in the reaction effluent.

The chemical industry reduces the impact on the environment during synthesis Methyl 2-cyano-2-methylpropanoate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; BASF SE; US2008/306299; (2008); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

New learning discoveries about 72291-30-6

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 2-cyano-2-methylpropanoate, its application will become more common.

Synthetic Route of 72291-30-6,Some common heterocyclic compound, 72291-30-6, name is Methyl 2-cyano-2-methylpropanoate, molecular formula is C6H9NO2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

To a solution of 122-1 (2.0 g, 15.73 mmol, 1 eq), (Boc)20 (6.87 g, 31.46 mmol, 7.23 mL, 2 eq) and NiCl2 (203.9 mg, 1.57 mmol, 0.1 eq) in MeOH (40 mL) at 0C was added NaBH4 (4.17 g, 110.11 mmol, 7 eq) slowly portion-wise, and the resulting mixture was stirred at 20C for 16 h. The reaction mixture was quenched with NH4.H20 (10 mL), and then concentrated to remove solvent. And the residue was diluted with water (50 mL), and then extracted with EA (50 mL *3). The combined organic layers were washed with brine (50 mL), dried over anhydrous Na2S04, filtered and concentrated under reduced pressure to give a residue. The residue was purified by flash silica gel chromatography to give 122-2 (600 mg, 2.59 mmol, 16.5% yield). 1H NMR (400 MHz, CDCI3) d 4.97 (brs, 1H), 3.69 (s, 3H), 3.24 (d, J= 6.6 Hz, 2H), 1.44 (s, 9H), 1.19 (s, 6H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 2-cyano-2-methylpropanoate, its application will become more common.

Reference:
Patent; VIVACE THERAPEUTICS, INC.; KONRADI, Andrei W.; LIN, Tracy Tzu-Ling Tang; (559 pag.)WO2019/222431; (2019); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Analyzing the synthesis route of 72291-30-6

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 2-cyano-2-methylpropanoate, its application will become more common.

Related Products of 72291-30-6,Some common heterocyclic compound, 72291-30-6, name is Methyl 2-cyano-2-methylpropanoate, molecular formula is C6H9NO2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

The reactant and the catalyst are initially charged in the autoclave and the contents are inertized by purging with nitrogen. Subsequently, 5 bar of hydrogen are injected. The desired amount of ammonia is metered in and then the autoclave is heated slowly with stirring to the reaction temperature (80 C.). This step takes an average of 90 min, i.e. the delay time of the reactant solution in contact with ammonia is approx. 90 min. On attainment of the reaction temperature, hydrogen is injected rapidly to the pressure specified in Table 1 below and consumed hydrogen is replaced by metering under pressure control over the experiment time until no further hydrogen absorption is recorded.The autoclave experiments are carried out in a 2.5 l autoclave with hollow-shaft disk stirrer (stirrer speed approx. 600 rpm), electrical heating and jacket air cooling, 2 baffles, sparging through the autoclave lid and introduction of the hydrogen via the hollow-shaft stirrer. The weights for Raney catalysts are corrected for 10% water moisture, i.e., in real terms, 10% more water-moist catalyst is weighed out than specified. Reaction effluents are analyzed via gas chromatography (GC) (conditions: 60 m DB1701; internal diameter 0.32 mm; film thickness 0.25 mum; detector: FID; temperature program: 80 C.?10 K/min?280 C., 40 min, split ratio 100:1, carrier gas helium) and the compositions are reported in % by weight.The reactor yield is determined by means of gas chromatography with internal standard (I.S.) (I.S. piperidine; the concentration thus obtained in the crude effluent is multiplied by the total mass of the crude effluent and the yield thus calculated is compared to the theoretical yield). The reactions are all carried out with methyl 2-cyano-2,2-dimethylacetate with a purity of >99.8%. The main product obtained is aminopivalinamide (3-amino-2,2-dimethylpropionamide). TABLE 1 Pressure/ % by weight ConcentrationNH3/ Purity Conversion Reactor Example bar Catalyst of catalyst Solvent % nitrile (crude, GC) % % yield % 1 200 Ra-Ni 10 NMP 30 20:1 98.7 100 not determined 2 65 Ra-Co 10 BuOH 40 7.7:1 98.8 100 94.0% 3 65 Ra-Ni 10 BuOH 40 7.7:1 98.2 99.7 90.6% 4 65 Ra-Ni 2.5 BuOH 40 3:1 93.7 99.7 84.9% 5 65 Ra0Co 2.5 BuOH 40 3:1 94.9 99.9 86.7 6 65 Ra-Co 5 MeOH 40 3:1 96.5 99.1 90.4 7 65 Ra-Co 5 MeOH 40 3:1 96.6 99.1 91.1 8 65 Ra-Co 5 BuOH 40 3:1 90.0 99.4 88.2 The examples show that very good selectivities of at least 90% are achievable with Raney nickel and Raney cobalt. The higher the amount of ammonia, the higher the catalyst concentration and the higher the hydrogen pressure, the better is the selectivity. In example 8, a metal determination is carried out, 430 ppm of Co are found in the reaction effluent.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 2-cyano-2-methylpropanoate, its application will become more common.

Reference:
Patent; BASF SE; US2008/306299; (2008); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts