14618-78-1 Archives - Nitriles-buliding-blocks

September 17, 2021 News Sources of common compounds: 14618-78-1

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4,4-Dimethoxybutanenitrile, and friends who are interested can also refer to it.

Related Products of 14618-78-1, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 14618-78-1 name is 4,4-Dimethoxybutanenitrile, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

In a 500 ml four-necked flask,Add 100 grams of tetrahydrofuran,13.0 g (0.1 mol) of 4,4-dimethoxy-n-butyronitrile,13.0 g (0.1 mol) of 2,3-dichloropropenal,0.5 g DBU,Reaction at 60 C for 4 hours,The gas phase detection 1,4-addition reaction is completed.Cool down to 25-30 C,Add 15.0 grams of potassium carbonate,25.0 grams of 17% ammonia,8.0 grams of ammonium chloride,Reaction at 50 C for 5 hours,Cool down to 20-25 C,filter,20 grams of ice water wash filter cake,dry,Obtained 13.5 g of 5-chloro-7-azaindole,The liquid phase purity is 99.7%,The yield was 88.5%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4,4-Dimethoxybutanenitrile, and friends who are interested can also refer to it.

Reference:
Patent; Xin Fa Pharmaceutical Co., Ltd.; Qi Yuxin; Zhang Mingfeng; Wang Sheng; Li Guangqian; Ju Lizhu; (7 pag.)CN110128421; (2019); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

13-Sep-21 News Discovery of 14618-78-1

The synthetic route of 14618-78-1 has been constantly updated, and we look forward to future research findings.

Synthetic Route of 14618-78-1, These common heterocyclic compound, 14618-78-1, name is 4,4-Dimethoxybutanenitrile, 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.

SYNTHESIS EXAMPLE 4 Production of methyl 4,5,7-trichloroindole-3-acetate: 10.0 Grams (0.047 mole) of 2,4,5-trichlorophenylhydrazine, 9.2 g (0.07 mole) of beta-cyanopropionaldehyde dimethylacetal and 7.1 g (0.052 mole) of zinc chloride were mixed and then heated in a nitrogen stream at 140 C. for 2 hours. The reaction mixture was cooled to room temperature and dissolved in an acetic acid-water (2:1) solution, and the resulting solution was extracted with ethyl acetate. The ethyl acetate phase was washed with a saturated aqueous sodium bicarbonate solution, water and then a saturated aqueous sodium chloride solution, and then dried over anhydrous sodium sulfate. The ethyl acetate was removed by distillation under reduced pressure to obtain a black oily substance, which was then purified by a silica gel column chromatography to obtained 0.86 g of the desired compound represented by the formula: STR15 The analysis result of NMR of this compound is shown below. 1 H NMR (200 MHz) (CD3)2 CO, TMS) ppm: 7.48 (1H, s).. C2 –H 7.34 (1H, s).. C6 –H 3.99 (2H, s).. CH2 — 3.66 (3H, s).. OCH3 MS (75 ev) (relative intensity, %) m/z 295 (M+ +4, 10), 293 (M+ +2, 23), 291 (M+, 24), 260 (6), 259 (5), 258 (7), 236 (30), 234 (91), 232 (100), 199 (7), 198 (9), 197 (11), 162 (12), 161 (13), 118 (7), 116 (8), 97 (9), 98 (9).

The synthetic route of 14618-78-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nippon Kayaku Kabushiki Kaisha; US4806143; (1989); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Extended knowledge of 14618-78-1

According to the analysis of related databases, 14618-78-1, the application of this compound in the production field has become more and more popular.

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 14618-78-1 as follows. name: 4,4-Dimethoxybutanenitrile

General procedure: One equiv. of carbazate was suspended in EtOH containing 10% (by vol.) of water(approx. 5 ml per mmol of the carbazate) and 1.05 equiv. of the acetal or ketal wasadded, followed by the addition of 0.05 equiv. of TFA. The reaction mixture was heatedto reflux and the progress of the reaction was monitored by TLC (thin layer chromatographyon silica gel) using ethyl acetate or a mixture of ethyl acetate-light petroleummixture (for the correct eluent, see characterization data of the compounds). After thereaction was complete, the reaction mixture was cooled to about 45C and three (3)equiv. of acetic acid was added, followed by the dropwise addition of a THF solutionof three (3) equiv. of NaBH3CN (approx. 1 ml of THF per 1.5 mmol of NaBH3CN).The reaction mixture was stirred at approx. 45C for 80 min. Subsequently, the reactionmixture was cooled to room temperature, acidified using 0.5 M HCl aqueous solution(6 ml of 0.5 M HCl per 1 mmol of starting carbazate) and stirred until the liberation ofhydrogen ceased. The reaction mixture was neutralized (to pH 8) by the dropwise additionof a saturated NaHCO3 solution (4 ml per 1 mmol of carbazate). The volatileswere removed under reduced pressure at approx. 40C. The residue was dissolved inethyl acetate, washed with saturated NaHCO3, twice with water and finally with saturatedaqueous sodium chloride. The combined aqueous washes were extracted twicewith ethyl acetate (25 ml per 1 mmol of expected product) and the extracts werewashed with saturated aqueous sodium chloride and combined with the organic phase. After drying over anhydrous Na2SO4 and evaporation of the solvent under reduced pressure,the residue was purified by column chromatography on silica gel using ethyl acetate-light petroleum (1:1 or 1:2) or ethyl acetate as eluent. For specific informationabout the eluent used to monitor the progress of the reaction and for purification, seethe Rf data for each compound.

According to the analysis of related databases, 14618-78-1, the application of this compound in the production field has become more and more popular.

Reference:
Article; Mastitski, Anton; Niinepuu, Siret; Haljasorg, Toiv; Jaerv, Jaak; Organic Preparations and Procedures International; vol. 47; 6; (2015); p. 490 – 498;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Sources of common compounds: 4,4-Dimethoxybutanenitrile

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4,4-Dimethoxybutanenitrile, and friends who are interested can also refer to it.

Synthetic Route of 14618-78-1, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 14618-78-1 name is 4,4-Dimethoxybutanenitrile, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4,4-Dimethoxybutanenitrile, and friends who are interested can also refer to it.

Continuously updated synthesis method about C6H11NO2

The synthetic route of 14618-78-1 has been constantly updated, and we look forward to future research findings.

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. 14618-78-1, name is 4,4-Dimethoxybutanenitrile, A new synthetic method of this compound is introduced below., HPLC of Formula: C6H11NO2

To a solution of diisopropylamine (4.77 mL, 34.1 mmol, 2.2 equiv) in THF (50 mL) at -10Cunder N2 was added 1.5 M n-BuLi in hexanes (22.7 mL, 34.1 mmol, 2.2 equiv). After 30 mm the mixturewas cooled to -78 C and a solution of nitrile (2.0 g, 15.5 mmol, 1.0 equiv) in THF (10 mL) was added.After 1 h iodomethane (2.12 mL, 34.1 mmol, 2.2 equiv) was added. The mixture was slowly warmed to 0C and kept there for 14 h, at which time it was quenched with sat. aq. NH4C1 (40 mL) and extracted withEtOAc (3 x 20 mL). The organics were dried over Na2SO4, filtered and concentrated in vacuo. Theresultant oil was purified by flash chromatography on silica gel (5:1 -3:1 hexanes/EtOAc) to yield theproduct (2.105 g, 87%) as a yellow oil. R1= 0.49 (3:1 hexanes/EtOAc). ?HNMR(400 MHz, CDC13) 3:4.60 (t, 1H, J= 5.6 Hz), 3.37 (s, 6H), 1.83 (d, 2H, J= 4.4 Hz), 1.39 (s, 6H); ?3C NMR (100 MHz, CDC13)3: 124.7, 102.4, 53.3, 43.0, 30.0, 27.5

The synthetic route of 14618-78-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SANFORD-BURNHAM MEDICAL RESEARCH INSTITUTE; SALK INSTITUTE FOR BIOLOGICAL STUDIES; PACHE, Lars; CHANDA, Sumit, K.; VAMOS, Mitchell, Dennis; COSFORD, Nicholas David, Peter; TERIETE, Peter; MARLETT, John; DIAZ, Arturo; YOUNG, John, A.T.; WO2015/187998; (2015); A2;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Discovery of 4,4-Dimethoxybutanenitrile

The synthetic route of 14618-78-1 has been constantly updated, and we look forward to future research findings.

Reference of 14618-78-1, These common heterocyclic compound, 14618-78-1, name is 4,4-Dimethoxybutanenitrile, 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 synthetic route of 14618-78-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Nippon Kayaku Kabushiki Kaisha; US4806143; (1989); A;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Discovery of 14618-78-1

The synthetic route of 14618-78-1 has been constantly updated, and we look forward to future research findings.

Electric Literature of 14618-78-1, A common heterocyclic compound, 14618-78-1, name is 4,4-Dimethoxybutanenitrile, molecular formula is C6H11NO2, 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.

Reference Example 68 2-formyl-4,4-dimethoxybutanenitrile Lithium diisopropylamide mono(tetrahydrofuran) (1.5 M in cyclohexane, 22.0 mL, 33.00 mmol) was added to THF (100 mL) at -30 C. and the resulting solution was stirred for 10 min before 3-cyanopropionaldehyde dimethyl acetal (3.90 mL, 29.90 mmol) was added dropwise over 5 min. After 15 min, methyl formate (2.80 mmol, 45.42 mmol) was added and the resulting solution was stirred at -20 C. to -15 C. for 2 h. The reaction mixture was quenched with water (100 mL) and washed with ether (2*50 mL, discarded). The aqueous layer was acidified with 10% HCl and extracted with ether (3*50 mL). The combined ether extracts were washed with brine (3*50 mL), dried (MgSO4), and concentrated. The residue was dissolved in dichloromethane and concentrated to remove traces of THF and provide 2.28 g (49%) of the title compound as a pale yellow oil.

The synthetic route of 14618-78-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Ortho-McNeil Pharmaceutical, Inc.; US6613747; (2003); B2;; ; Patent; Henninger, Todd C.; Xu, Xiaodong; US2002/115620; (2002); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Brief introduction of 4,4-Dimethoxybutanenitrile

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4,4-Dimethoxybutanenitrile, and friends who are interested can also refer to it.

As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 14618-78-1 name is 4,4-Dimethoxybutanenitrile, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. 14618-78-1

In a 500 ml four-necked flask,Add 60 grams of DMF,13.0 g (0.1 mol) of 4,4-dimethoxy-n-butyronitrile,10.0 g (0.11 mol) of 2,3-difluoropropenal,0.8 g DBU, reacted at 80 C for 5 hours,The gas phase detection 1,4-addition reaction is completed.Cool down to 25-30 C,Add 10.0 grams of potassium carbonate,22.0 grams of 17% ammonia,10.0 g of ammonium chloride,Reaction at 80 C for 4 hours,Cool down to 20-25 C,filter,20 grams of ice water wash filter cake,dry,Obtained 11.4 g of 5-fluoro-7-azaindole,Liquid phase purity is 99.2%,The yield was 83.8%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4,4-Dimethoxybutanenitrile, and friends who are interested can also refer to it.