HRID40712

反应详情

EQUATION

反应方程式

HRID 40712 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

1.0 g (4.04 mmol) of N-(5-acetyl-2-chloro-phenyl)-methanesulfonamide were dissolved in 10 ml of dry N,N-dimethylformamide and 2.69 ml (2.41 g) (20.19 mmol) of N,N-dimethylformamide dimethylacetal. The resultant solution was refluxed for 2 hours. The solvent and the excess of volatile reagent was removed by reduced pressure distillation to yield an oil which, in the presence of ethyl acetate, gave 1.04 of a crude. It was chromatographied (silica gel) using ethyl acetate/2-propanol as eluent. 0.51 g of N-[2-chloro-5-(3-dimethylamino-acryloyl)-phenyl]-N-methyl-methanesulfonamide as a yellowish-white solid were obtained (yield 40%).

WORKUP

后处理

  1. customThe solvent and the excess of volatile reagent was removed by reduced pressure distillation
  2. customto yield an oil which