HRID482261

反应详情

EQUATION

反应方程式

HRID 482261 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7.12 g (30 mmol) of 1-amidino-4,4-dimethyl-2-oxoimidazolidine hydrobromide were added to a mixture of 70 ml of 1-propanol and 5.5 ml of a 30% strength solution of sodium methylate in methanol (=30 mmol) at room temperature, and the mixture was stirred at room temperature for 20 min. Subsequently, at 20° C., 8.95 g (30 mmol) of 2-cyano-3-ethoxyacrylic acid N-methyl-N-(3-trifluoromethylphenyl)amide were added, and the mixture was stirred at 20° C. for 30 min and at 20°-25° C. for 1.5 hours. The solid which had separated out was then filtered off with suction, washed with 1-propanol and with water and dried as described in Example 1. The original filtrate was worked up as in Example 1. 6.82 g (=55.7% yield) of, according to TLC, virtually pure compound IV were obtained.

WORKUP

后处理

  1. stirringthe mixture was stirred at 20° C. for 30 min and at 20°-25° C. for 1.5 hours
  2. customThe solid which had separated out
  3. filtrationwas then filtered off with suction
  4. washwashed with 1-propanol and with water
  5. customdried