Category: 7341-96-0

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. 7341-96-0, name is Propiolamide, A new synthetic method of this compound is introduced below., HPLC of Formula: C3H3NO

Aimine (0.24 mmol)Rhodium acetate (0.0024 mmol) and molecular sieves (300 mg) were mixed in 10 mL single-necked vials,Oil pump for nitrogen ventilation,A 1 mL syringe was added with 1 mL of re-evaporated CH? Cl?Prepared as a mixed solution A and stirred at room temperature for 10 minutes.The aryl diazonium compound (0.2 mmol) and the amide compound (0.2 mmol) were dissolved in 1 mL of re-evaporated CH? Cl?Prepared into solution B. Solution B was added to the mixed solution A at 25 C with a syringe pump over 1 hour.Stirring for 3 to 12 hours, the reaction mixture is purified by column chromatography to obtain a pure product,Its structure as shown in equation (f)(2S, 3S) -3- (4-trifluoromethylphenyl) -3 – ((2-hydroxyphenyl) amino) -2-phenyl-2-propiolamide propionate,The yield was 70%Dr value is equal to 95: 5, HPLC purity is 97%.

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; East China Normal University; Liu Shunying; Lei Ruirui; Jia Kaili; Wu Yong; Liu Donglan; Dong Suzhen; Hu Wenhao; (42 pag.)CN106831474; (2017); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 7341-96-0, 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. 7341-96-0, name is Propiolamide belongs to amides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

The imine (0.2mmol), rhodium acetate (0.002mmol), Molecular sieve (300 mg) and the mixture is dissolved 1.5 ml dichloromethane solvent, into mixed solution 1, in 20 C stirring for 10 minutes. Then the propargyl amide (0.24mmol) and phenyl diazonium acetic acid methyl ester (0.24mmol) dissolved in 1.0 ml methylene chloride solvent, into solution 2. The solution 2 for 20 C lower, in 1 hour for adding and mixing the solution in the injection pump 1. The reaction mixture is purified by rapid column chromatography, to obtain the pure product, its structure is shown as formula (f) is shown. The yield is 89%, dr value is equal to the 88:12. The product of the1As shown in Figure 11, H NMR schematic view thereof13C NMR schematic view as shown in Figure 12.

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, Propiolamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; EAST CHINA NORMAL UNIVERSITY; HU, WENHAO; WU, YONG; WANG, WENKE; TANG, MIN; (29 pag.)CN106146334; (2016); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 7341-96-0, 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 7341-96-0 as follows.

To a cooled (0 C), clear, yellow solution of 4-chloro-3-fluoro-2-(6- methoxypyrimidin-4-yl)aniline (1 g, 3.94 mmol) in ACN (56.3 ml) was added isoamylnitrite (0.79 ml, 5.91 mmol), followed by the dropwise addition of TMSN3 (0.79 ml, 5.91 mmol). After 10 mm, the cold bath was removed, and the reaction was allowed to warm to rt and stirred at rt for lh. Next, propiolamide (0.8 17 g, 11.83 mmol) andCu20 (0.05 6 g, 0.3 94 mmol) were added. After 1 h, the yellow cloudy reaction was diluted with EtOAc, and washed with sat NH4C1, brine, dried over MgSO4, filtered and concentrated to give a yellow solid. DCM (10 ml) was added and the resulting mixture was sonicated. The suspension was filtered and the solid was air-dried. A yellow solid obtained as 1 -(4-chloro-3 -fluoro-2-(6-methoxypyrimidin-4-yl)phenyl)- 1 H- 1,2,3 -triazole25 4-carboxamide (1.003 g, 73.0% yield). MS(ESI) m/z: 349.0 (M+H).

According to the analysis of related databases, 7341-96-0, the application of this compound in the production field has become more and more popular.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; CORTE, James R.; DE LUCCA, Indawati; FANG, Tianan; YANG, Wu; WANG, Yufeng; DILGER, Andrew K.; PABBISETTY, Kumar Balashanmuga; EWING, William R.; ZHU, Yeheng; WEXLER, Ruth R.; PINTO, Donald J. P.; ORWAT, Michael J.; SMITH, Leon M. II; WO2015/116886; (2015); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Synthetic Route of 7341-96-0, These common heterocyclic compound, 7341-96-0, name is Propiolamide, 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.

Example 2.1: Ethyl 2-{2-ethoxy-2-oxoethyl)-6-oxo-1,6-dihydropyridine-3- cartooxylate; Propiolamide (20.0 g, 289.6 mmol), diethyl 3-oxopentanedioate (87.8 g, 434.4 mmol) and sodium carbonate (24.6 g, 231.7 mmol) were mixed in water (800 mL) at 0 0C and then warmed to r.t. over 4 hours. The reaction was allowed to continue t? stir at r.t. for 3 days. The reaction was neutralized with aqueous hydrochloric acid (5M) at 0 0C with vigorous stirring. A solid precipitate was collected by filtration and washed with diethyl ether/hexanes (2:1) to yield a first batch of the title compound (43g). The filtrate was further extracted with ethyl acetate and the combined organic phases were dried over sodium sulphate and purified by column chromatography (10-80% ethyl acetate/hexanes) to yield another batch of the title compound (7g), in total gave 50 g (68%). 1H NMR (300 MHz, CDCI3): delta(ppm) 13-12 (br S, 1 H)1 8.08 (d, 1H), 6.52 (d, 1H), 4.3 (q, 2H), 4.21 (q, 2H)1 4.13 (s, 2H)1 1.29 (m, 6H).

Statistics shows that Propiolamide is playing an increasingly important role. we look forward to future research findings about 7341-96-0.

Reference:
Patent; NPS ALLELIX CORP.; WO2008/9125; (2008); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

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. 7341-96-0, name is Propiolamide, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 7341-96-0

The imine (0.2mmol), rhodium acetate (0.002mmol), Molecular sieve (300 mg) and the mixture is dissolved 1.5 ml dichloromethane solvent, into mixed solution 1, in 20 C stirring for 10 minutes. Then the propargyl amide (0.24mmol) and methoxyphenyl diazo acetic acid methyl ester (0.24mmol) dissolved in 1.0 ml methylene chloride solvent, into solution 2. The solution 2 for 20 C lower, in 1 hour for adding and mixing the solution in the injection pump 1. The reaction mixture is purified by rapid column chromatography, to obtain the pure product, its structure is formula (d) is shown. The yield is 81%, dr value equal to 90:10. The product of the1As shown in Figure 7, H NMR schematic view thereof13C NMR schematic view as shown in Figure 8.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 7341-96-0.

Reference:
Patent; EAST CHINA NORMAL UNIVERSITY; HU, WENHAO; WU, YONG; WANG, WENKE; TANG, MIN; (29 pag.)CN106146334; (2016); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Electric Literature of 7341-96-0,Some common heterocyclic compound, 7341-96-0, name is Propiolamide, molecular formula is C3H3NO, 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 imine (0.2mmol), rhodium acetate (0.002mmol), Molecular sieve (300 mg) and the mixture is dissolved 1.5 ml dichloromethane solvent, into mixed solution 1, in 20 C stirring for 10 minutes. Then the propargyl amide (0.24mmol) and phenyl diazonium acetic acid methyl ester (0.24mmol) dissolved in 1.0 ml methylene chloride solvent, into solution 2. The solution 2 for 20 C lower, in 1 hour for adding and mixing the solution in the injection pump 1. The reaction mixture is purified by rapid column chromatography, to obtain the pure product, its structure is shown as formula (g) is shown. The yield is 89%, dr value is equal to the 88:12. The product of the1As shown in Figure 13, H NMR schematic view thereof13C NMR schematic view as shown in Figure 14.

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

Reference:
Patent; EAST CHINA NORMAL UNIVERSITY; HU, WENHAO; WU, YONG; WANG, WENKE; TANG, MIN; (29 pag.)CN106146334; (2016); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

Application of 7341-96-0, A common heterocyclic compound, 7341-96-0, name is Propiolamide, molecular formula is C3H3NO, 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.

A solution of 4-(tert-butyl-dimethyl-silanyloxymethyl)-benzaldehyde oxime (which may be made as described in Preparation of Intermediate 17; 3 g, 11.3 mmol) in DMF (25 mL) was cooled to 0 C and N-chlorosuccinimide (1.51 g, 11.3 mmol) was added in portions. The cooling bath was removed and the reaction mixture was stirred for 2.5 h. The mixture was poured into ice- water (75 mL) and this was extracted with Et2O (3 x 100 mL). The combined organic layers were washed with brine, dried (Na2SO4) and evaporated to give a solid (3.5 g). The solid was dissolved in 50% aqueous tert-butanol (60 mL) in a flask that was open to the air. Propiolamide (which may be prepared as described in Matsumoto, T. et al. US 7,851,473 Column 128; 0.7 mL, 6.85 mmol) was added, followed by 1 M sodium ascorbate (1.13 mL, 1.13 mmol) and 0.1 M copper(II) sulfate (5.65 mL, 0.565 mmol). KHCO3 (4.52 g, 45.1 mmol) was added in portions and the reaction mixture was stirred at room temperature for 2.5 h. H2O (100 mL) was added and a yellow solid was filtered off and dried under high vacuum overnight (3 g). This material was taken up in CH2Cl2/acetone and filtered. The filtrate was evaporated and the residue was purified by chromatography (9-20% acetone/CH2Cl2) to give 3-[4-(tert-butyl-dimethyl- silanyloxymethyl)-phenyl]-isoxazole-5-carboxylic acid amide (800 mg, 21%). Purification of mixed fractions by chromatography (50-60% EtO Ac/toluene) provided a further 450 mg (12%) of 3-[4-(tert-butyl-dimethyl-silanyloxymethyl)-phenyl]-isoxazole-5-carboxylic acid amide.

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; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; ERICKSON, Shawn, David; GILLESPIE, Paul; MERTZ, Eric; WO2014/86704; (2014); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

These common heterocyclic compound, 7341-96-0, name is Propiolamide, 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. 7341-96-0

Aimine (0.24 mmol)Rhodium acetate (0.0024 mmol) and molecular sieves (300 mg) were mixed in 10 mL single-necked vials,Oil pump for nitrogen ventilation, with 1mL syringe by adding 1mL re-steamed CH2Cl2 solution, prepared into a mixed solution A,And the mixture was stirred at room temperature for 10 minutes.The aryl diazonium compound (0.2 mmol) and the amide compound (0.2 mmol) were dissolved in 1 mL of re-evaporated CH2Cl2 To prepare solution B. Solution B was added to the mixed solution A at 25 C with a syringe pump over 1 hour. The mixture is stirred for 3 to 12 hours and the reaction mixture is purified by column chromatography to give pure product as shown in formula (k)For methyl(2S, 3S) -3- (4-bromophenyl) -3 – ((2-hydroxyphenyl) amino) -2- (4-chlorophenyl) -2-propiolamide propionate Rate of 70%Dr value equal to> 95: 5, HPLC purity is 95%.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 7341-96-0.

Reference:
Patent; East China Normal University; Liu Shunying; Lei Ruirui; Jia Kaili; Wu Yong; Liu Donglan; Dong Suzhen; Hu Wenhao; (42 pag.)CN106831474; (2017); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

7341-96-0, The chemical industry reduces the impact on the environment during synthesis 7341-96-0, name is Propiolamide, I believe this compound will play a more active role in future production and life.

The imine (0.2mmol), rhodium acetate (0.002mmol), Molecular sieve (300 mg) and the mixture is dissolved 1.5 ml dichloromethane solvent, into mixed solution 1, in 20 C stirring for 10 minutes. Then the propargyl amide (0.24mmol) and phenyl diazonium acetic acid methyl ester (0.24mmol) dissolved in 1.0 ml methylene chloride solvent, into solution 2. The solution 2 for 20 C lower, in 1 hour for adding and mixing the solution in the injection pump 1. The reaction mixture is purified by rapid column chromatography, to obtain the pure product, its structure is formula (b) is shown. The yield is 87%, dr value is equal to the 89:11.

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

Reference:
Patent; EAST CHINA NORMAL UNIVERSITY; HU, WENHAO; WU, YONG; WANG, WENKE; TANG, MIN; (29 pag.)CN106146334; (2016); A;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics

7341-96-0, A common compound: 7341-96-0, name is Propiolamide, belongs to amides-buliding-blocks compound, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below.

Example 6; Synthesis of compound (I): 1-(2,6-Difluorobenzyl)-1H-1,2,3-triazole-4-carboxyamide (Rufinamide) A 500 ml round-bottom flask is loaded with 2,6-difluorobenzyl azide (100 g, 0.59 mole) dissolved in methanol (300 ml), then propiolamide (49 g, 0.71 mole) obtained according to Example 5 is added under stirring to obtain a solution. Afterwards, CuSO4 pentahydrate (1.46 g, 5.9 mmoles) and ascorbic acid (5.19 g, 29.6 mmoles) are added in succession. The reaction mixture spontaneously reaches 40C and is kept under stirring for 4 hours at the same temperature. The formed solid is then filtered off, washed with methanol and water, and dried in an oven at 50C, thereby affording 133 g of a solid crude in 89% yield. The solid is suspended in water (300 ml), the suspension is treated with 33% aqueous ammonia (50 ml) and left under stirring for 3 hours, then the resulting white solid is filtered and dried in an oven. 130 g of a crystalline solid are obtained in 87% yield. 1H NMR (400 MHz, DMSO-d6), delta ppm: 8.56 (s, 1 H), 7.87 (bs, 1H), 7.60-7.43 (m, 2H), 7.20 (m, 2H), 5.72 (s, 2H).

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, Propiolamide, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Dipharma Francis S.r.l.; EP2230234; (2010); A1;,
Amide – Wikipedia,
Amide – an overview | ScienceDirect Topics