Category: 103146-25-4

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 103146-25-4 as follows. Safety of 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile

A four-necked flask equipped with stirrer and thermometer was charged with 250.0 g of a solution of 25.0 g (0.073 mol) of [()-4- [4-DIMETHYLAMINO-L- (4′-FLUOROPHENYL)-L-] hydroxybutyl] -3-hydroxymethylbenzonitrile in toluene, and the temperature thereof was controlled so as to be [40C.] Then, 5.77 g (0.073 mol) of pyridine, 8.33 g (0.073 mol) of vinyl butyrate, 9.93 g (0.073 mol) of o-toluic acid, and 5.0 g of an immobilized enzyme (Novozym 435) was added into the above mixture. The reaction mixture was stirred at [40C] for 21 hours under a slight flow of nitrogen, and then stirring was stopped. The enzyme was filtrated from the reaction mixture with Kiriyama [FUNNEL,] and washed with 54.1 g of toluene. As a result, a toluene layer containing (S)-4- [4-dimethylamino-1- (4′-fluorophenyl)-1-hydroxybutyl]- 3-hydroxymethylbenzonitrile (9.7 g, 0. [028] mol, yield: 38.8%, optical purity: 97.8% ee), o-toluic acid salt was obtained. The combined toluene layer was washed three times with water (250 ml, 63 ml, 63 ml) at [60C,] and an aqueous layer containing [(S)-4- [4-DIMETHYLAMINO-L- (4′-] [FLUOROPHENYL)-L-HYDROXYBUTYL]-3-LIYDROXYMETHYLBENZONITRILE] (7.8 g, 0.0228 mol, extraction yield: 80%), o-toluic acid salt was obtained.

According to the analysis of related databases, 103146-25-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; H. LUNDBECK A/S; WO2004/14821; (2004); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

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. 103146-25-4, name is 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. HPLC of Formula: C20H23FN2O2

R-enriched cyanodiol (lOg, 0.029 moles) was dissolved in MDC (30ml) at 20-40 C. To the obtained clear reaction mass imidazole (5.96g, 0.0438 moles) followed by a solution of t-butyldimethylsilylchloride (TBDMSC1) (6.60g, 0.04 moles) in dichloromethane (10ml) was added at 20-40 C and the reaction mass stirred further at 20-30C for 1-2 hours. Then the reaction mass was directly washed with water (30ml x 3) after which the lower organic layer was separated and concentrated under vacuum at 35-40 C which yielded l l .Ogm title compound ( lib) as a off white solid. 1H-NMR in DMSO at 300MHz (ppm):0.23-0.24 (d,3H), 0.17-0.18(d,3H), 0.76- 0.77 (s, 9H), 0.83-0.85 (d, lH), 1.17-1.22 (m,lH), 1.41-1.45 (m,lH), 2.03 (s,6H), 2.08-2.25 (m,4H), 4.27-4.33 (dd,lH), 4.74-4.79 (dd,lH), 7.07-7.13 (t,2H), 7.23- 7.27 (m,2H),7.80-7.83 (d,3H) FT-IR as such (cm”1): 2952, 2855, 2227, 1599, 1506, 1470, 1253, 1216, 1160, 1122, 1109, 1092, 1035, 1016, 958, 897 Mass Analysis (ESI, +ve mode): Molecular ion peak observed at 457.47 a.m.u which corresponds to (M+H)+ peak of title compound DSC Analysis: Two Endotherm peaks observed at 124.89 and 136.30 C XRPD Analysis (Observed 2Theta values):8.09, 9.32, 10.45, 11.44, 12.34, 13.29, 14.02, 15.57, 16.26, 16.87, 17.51, 18.18, 18.71, 19.34, 19.87, 20.39, 20.99, 21.47, 22.13, 22.49, 23.01, 23.29, 24.49, 24.87, 25.33, 25.74, 26.29, 26.78, 27.03, 27.52, 28.26, 28.69, 29.05, 29.41, 29.61, 30.13, 31.44, 32.09, 32.37, 32.86, 33.17, 33.77, 34.78, 35.16, 35.81, 36.74, 37.54, 38.33, 38.64, 39.45, 40.16, 41.24, 41.59, 42.24, 43.03, 44.29, 45.79, 47.81, 48.49 Purity by HPLC : 91 27%

The synthetic route of 103146-25-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; IPCA LABORATORIES LIMITED; REGURI, Buchi Reddy; PRASAD, Ashok; RAWAT, Ajay Singh; RAJPUT, Sandip; SANTAN, Rohit B; (36 pag.)WO2017/9866; (2017); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 103146-25-4, name is 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile, belongs to nitriles-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 103146-25-4, category: nitriles-buliding-blocks

Experiment 7; The general procedure of Experiment 2 was applied. No acetic acid was present in the system. The experiment was carried out with a small amount of water (0.01V)An exemplary batch gave molar yield: 32.5%; enantiomeric purity: 98.7% S.; Experiment 8; The general procedure of Experiment 2 was applied. No acetic acid was present in the system. The experiment was carried out with a higher amount of water (0.05V)Exemplary batches gave:Molar yield: 34.7%; enantiomeric purity: 99.0% S.; Experiment 9; The general procedure of Experiment 2 was applied. Additionally a small amount of water (0.05 V) was added to the 4-[4-(dimethylamino)-1-(4′-fluorophenyl)-1-hydroxybutyl]-3-(hydroxymethyl)-benzonitrile free base solution in 1-propanol.An exemplary batch gave molar yield: 33.0%; enantiomeric purity: 99.1% S.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it.

Reference:
Patent; H. Lundbeck A/S; US2009/69582; (2009); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

These common heterocyclic compound, 103146-25-4, name is 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile, 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: 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile

Experiment 4; The general procedure of Experiment 2 was applied. To the 4-[4-(dimethylamino)-1-(4′-fluorophenyl)-1-hydroxybutyl]-3-(hydroxymethyl)-benzonitrile free base solution in 1-propanol was added 0.05 V of water. No toluene or acetic acid was present in the system.An exemplary batch gave molar yield: 29.3%; enantiomeric purity: 99.3% S.

The synthetic route of 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile has been constantly updated, and we look forward to future research findings.

Reference:
Patent; H. Lundbeck A/S; US2009/69582; (2009); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 103146-25-4, name is 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile, belongs to nitriles-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 103146-25-4, Safety of 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile

Experiment 4: The general procedure of Experiment 2 was applied. To the 4-[4-(dimethylamino)- l-(4′-fluorophenyl)-l-hydroxybutyl]-3-(hydroxymethyl)-benzonitrile free base solution in 1-propanol was added 0.05 V of water. No toluene or acetic acid was present in the system. An exemplary batch gave molar yield: 29.3%; enantiomeric purity: 99.3% S.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile, and friends who are interested can also refer to it.

Reference:
Patent; H. LUNDBECK A/S; WO2009/33488; (2009); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Reference of 103146-25-4, 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. 103146-25-4, name is 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile belongs to nitriles-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A four-necked flask equipped with stirrer and thermometer was charged with 219 g of a solution containing 21.9 g (0.064 mol) of [()-4- [4-DIMETHYLAMINO-L-] (4′- [FLUOROPHENYL)-1-HYDROXYBUTYL]-] 3-hydroxymethylbenzonitrile in toluene. Then, 14.6 g (0.128 mmol) of vinyl butyrate, 5.07 g (0.128 mol) of pyridine, 7.89 g (0.064 mol) of benzoic acid and 2.19 g of an immobilized enzyme (Novozym 435) were added into the above mixture. The reaction mixture was allowed to warm up to [60 C] and stirred for 15 hours under a slight flow of nitrogen and stirring was stopped. The enzyme was filtrated off from the reaction mixture with Kiriyama funnel, and washed with 50 g of toluene. The combined toluene layer was washed twice with water (255 ml, 265 ml) and concentrated to give 14.9 g of [(R)-5-CYANO-2-] [dimethylamino- (4′-fluorophenyl)- hydroxybutyl] benzyl butyrate benzoic acid salt. To a mixture of 4.0 g of (R) -5-Cyano-2- [dimethylamino- (4′-fluorophenyl)- hydroxybutyl] benzyl butyrate benzoic acid salt (7.48 mmol), 40 ml of water and 40 ml of toluene were added 1.26 g of 30% sodium hydroxide (9.45 mol) with stirring, the mixture was kept stirring for 30 minutes. After stirring, the mixture was allowed to stand and the toluene layer was separated. The toluene layer was washed with 40 ml of water and concentrated at [40 C] under reduced pressure, to thereby obtain 2.7 g of (R) -5-Cyano-2- [dimethylamino- [(4′-FLUOROPHENYL)-HYDROXYBUTYL]] benzyl butyrate. 1H NMR (400 MHz. CDC13) [A] (ppm): 7.69 [(1H,] s), 7.68-7. 56 (2H, m), 7.36-7. 23 (2H, m), 7.02-6. 90 (2H, m), 5.41 [(1H,] d, J [14.] 9 Hz), 4.99 [(1H,] d, J [14.] 6 Hz), 2.59- 2.42 [(1H,] m), 2.40-2. 30 (3H, m), 2.26 (2H, dt, J= 7.3 Hz, 1.5 Hz), 2.18 (6H, s), 1.68- 1.57 (2H, m), 1.67-1. 46 (2H, m), 0.93 (3H, t, [J =] 7.6 Hz).

The synthetic route of 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile has been constantly updated, and we look forward to future research findings.

Reference:
Patent; H. LUNDBECK A/S; WO2004/14821; (2004); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

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. 103146-25-4, name is 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile, A new synthetic method of this compound is introduced below., SDS of cas: 103146-25-4

In a 200-ml four-necked flask equipped with a stirrer and a thermometer, 1.5 g [(4.] [38] m mol) of [()-4- [4-DIMETHYLAMINO-1- (4′-FLUOROPHENYL)-1-HYDROXYBUTYL]-3-] hydroxymethylbenzonitrile was dissolved in 30 ml of toluene, then 0.45 g of Novozym 435 (product [OF NOVOZYMES),] 0.347 g (4.38 m mol) of pyridine, 4.38 m mol of various kinds of acids and 1.00 g (8.76 m mol) of vinyl butyrate were added, and stirred at [40C] for between 16 and 21.5 hours. The result is shown in Table 4. Example 6 In a 200-ml four-necked flask equipped with a stirrer and a thermometer, 3.0 g [(8.] 76 m mol) of [( : L)-4- [4-DIMETLIYLAMINO-L- (41-FLUOROPHENYL)-L-HYDROXYBUTYL]-3-] hydroxymethylbenzonitrile was dissolved in 30 ml of toluene, then 0.9 g of Novozym [435] (product [OF NOVOZYMES),] 0.693 g (8.76 m mol) of pyridine, 8.76 m mol of various kinds of acids and 2.00 g (17.52 m mol) of vinyl butyrate were added, and stirred at [40C] for between 15.5 and 16.5 hours. The results are shown in Table 5.

The synthetic route of 103146-25-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; H. LUNDBECK A/S; WO2004/14821; (2004); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Some common heterocyclic compound, 103146-25-4, name is 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile, molecular formula is C20H23FN2O2, 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: 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile

Experiment 7: The general procedure of Experiment 2 was applied. No acetic acid was present in the system. The experiment was carried out with a small amount of water (0.0 IV) An exemplary batch gave molar yield: 32.5%; enantiomeric purity: 98.7% S. Experiment 8: The general procedure of Experiment 2 was applied. No acetic acid was present in the system. The experiment was carried out with a higher amount of water (0.05V) Exemplary batches gave: Molar yield: 34.7%; enantiomeric purity: 99.0% S.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 103146-25-4, its application will become more common.

Reference:
Patent; H. LUNDBECK A/S; WO2009/33488; (2009); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

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. 103146-25-4, name is 4-(4-(Dimethylamino)-1-(4-fluorophenyl)-1-hydroxybutyl)-3-(hydroxymethyl)benzonitrile, A new synthetic method of this compound is introduced below., category: nitriles-buliding-blocks

A four-necked flask equipped with stirrer and thermometer was charged with 250.0 g of a solution of 50.0 g (0.146 mol) of ()-4- [4-dimethylamino-l- (4′-fluorophenyl)-l- hydroxybutyl] -3-hydroxymethylbenzonitrile in toluene, and the temperature thereof was controlled so as to be [40C.] Then, 11.5 g (0.146 mol) of pyridine, 33.2 g (0.291 mol) of vinyl butyrate, 17.8 g (0.146 mol) of benzoic acid, and 10.0 g of an immobilized enzyme (Novozym 435) was added into the above mixture. The reaction mixture was stirred at [40C] for 20 hours under a slight flow of nitrogen, and then stirring was stopped. The enzyme was filtrated from the reaction mixture with Kiriyama funnel, and washed with 108 g of toluene. As a result, a toluene layer containing [(S)-4- [4-DIMETHYLAMINO-1- (4′-FLUOROPHENYL)-1-HYDROXYBUTYL]-] 3-hydroxymethylbenzonitrile (22.0 g, 0.064 mol, yield: 44.0%, optical purity: 99.0% [EE),] benzoic acid salt was obtained. The combined toluene layer was washed three times with water (500 ml x 3) at [60C,] and an aqueous layer containing [(S)-4- [4-DIMETHYLAMINO-L- (4′-FLUOROPHENYL)-L-] hydroxybutyl]-3-hydroxymethylbenzonitrile (21.0 g, 0.0614 mol, extraction yield: 96%), benzoic acid salt was obtained.

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; H. LUNDBECK A/S; WO2004/14821; (2004); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts

Electric Literature of 103146-25-4, 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 103146-25-4 as follows.

Experiment 9: The general procedure of Experiment 2 was applied. Additionally a small amount of water (0.05 V) was added to the 4-[4-(dimethylamino)-l-(4′-fluorophenyl)- l-hydroxybutyl]-3-(hydroxymethyl)-benzonitrile free base solution in 1-propanol. An exemplary batch gave molar yield: 33.0%; enantiomeric purity: 99.1% S.

According to the analysis of related databases, 103146-25-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; H. LUNDBECK A/S; WO2009/33488; (2009); A1;,
Nitrile – Wikipedia,
Nitriles – Chemistry LibreTexts