HRID2089683

反应详情

EQUATION

反应方程式

HRID 2089683 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A mixture of the crude product containing carbonic acid {3-[1-(4-cyanophenylimino)-2-methoxycarbonylimino-2-methylsulfanylethyl]-2-fluoro-5-methoxyphenoxy}ethyl ester methyl ester (37 g, 73.4 mmol), toluene (740 mL), pyrimidin-2-yl-hydrazine (8.08 g, 73.4 mmol), and triethylamine (12.3 mL, 88.2 mmol) was heated at 50° C. for 10 minutes under stirring, gradually heated to 110° C., and heated at 110° C. for 4 hours under stirring. The mixture was gradually cooled to room temperature, and then the precipitate was filtered and dried to obtain the captioned compound (23.89 g) as a pale yellow powder.

WORKUP

后处理

  1. temperaturegradually heated to 110° C.
  2. temperatureheated at 110° C. for 4 hours
  3. stirringunder stirring
  4. temperatureThe mixture was gradually cooled to room temperature
  5. filtrationthe precipitate was filtered
  6. customdried