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.
N-Chlorosuccinimide (624 mg, 4.7 mmol) was added in portions to a solution of 4- bromomethyl-benzaldehyde oxime (which may be prepared as described in Charrier, J.-D. et al. WO2011/143426 p 77; 1 g, 4.7 mmol) in DMF (9 mL) at room temperature. The reaction mixture was stirred for 2 h under argon. The mixture was poured into ice-water and this was extracted with Et2O (3 x 50 mL). The combined organic layers were washed with brine, dried (Na2SO4) and evaporated to give a solid (1.4 g). The solid was dissolved in 50% aqueous tert-butanol (20 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; 323 mg, 4.7 mmol) was added, followed by 1 M sodium ascorbate (0.47 mL, 0.47 mmol) and 0.1 M copper(II) sulfate (2.34 mL, 0.23 mmol). KHCO3 (1.87 g, 18.7 mmol) was added in portions and the reaction mixture was stirred at room temperature for 3 h. H2O (25 mL) was added and the mixture was extracted with 85: 15 CHCl3/CH3OH (3 x 100 mL). The combined organic layers were washed with brine, dried (Na2S04), filtered, evaporated, and purified by chromatography (16-20% acetone/CH2Cl2) to give 3-(4-bromomethyl- phenyl)-isoxazole-5-carboxylic acid amide (156 mg, 12%). Purification of mixed fractions by chromatography (16-20% acetone/CH2Cl2) provided a further 40 mg (3%) of 3-(4- bromomethyl-phenyl)-isoxazole-5-carboxylic acid amide.
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; F. HOFFMANN-LA ROCHE AG; HOFFMANN-LA ROCHE INC.; ERICKSON, Shawn, David; GILLESPIE, Paul; MERTZ, Eric; WO2014/86704; (2014); A1;,
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