HRID623830
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customReaction completion
- customReaction mixture
- concentrationwas concentrated under reduced pressure