HRID623830

反应详情

EQUATION

反应方程式

HRID 623830 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

In a 3-neck 100 mL round-bottomed flask, 3-cyano-5-(trifluoromethyl)benzoic acid (2.5 g, 1 eq.) was dissolved in dichloromethane (25 mL, 10 Vol) and cool to 0° C. added DMF (0.2 mL, cat.). Then added oxalyl chloride drop wise in 0.5 hr. The reaction mixture was stirred at 0° C. for 1-2 hr. Reaction completion was monitored on TLC using MeOH:dichloromethane (1:9) mobile phase. Reaction mixture was concentrated under reduced pressure to afford 3.0 g of crude 3-cyano-5-(trifluoromethyl)benzoyl chloride, which was immediately used for next step.

WORKUP

后处理

  1. customReaction completion
  2. customReaction mixture
  3. concentrationwas concentrated under reduced pressure