HRID1861214

反应详情

EQUATION

反应方程式

HRID 1861214 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

1.4 g (0.01 mol) of ethyl 3-dimethylaminoacrylate, 15 ml of ethyl acetate and 1.4 ml (0.01 mol) of triethylamine were loaded and cooled to 5° C., and a liquid mixture of 3.5 g (0.011 mol) of 2,4,5-trifluoro-3-methyl-6-nitrobenzoyl chloride and 5 ml of ethyl acetate was added dropwise while the temperature was maintained at 0 to 5° C. The resulting mixture was stirred at 5° C. for 1 hour and then stirred at room temperature (25° C.) for 2 hours. The precipitated triethylamine hydrochloride was filtered off, and the filtrate was concentrated under reduced pressure to give ethyl 3-dimethylamino-2-(2,4,5-trifluoro-3-methyl-6-nitrobenzoyl)acrylate with a 43.6% purity as the residue.

WORKUP

后处理

  1. additionwas added dropwise while the temperature
  2. temperaturewas maintained at 0 to 5° C
  3. stirringstirred at room temperature (25° C.) for 2 hours
  4. filtrationThe precipitated triethylamine hydrochloride was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure