HRID639626

反应详情

EQUATION

反应方程式

HRID 639626 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Ethyl-[2-chloro-3-nitro-6-(trifluoromethyl)-pyridin-4-yl]-benzylcarbamate (63 gm 160 mmol) was dissolved in tetrahydrofuran (300 mL) and to this was added 0.880 ammonia solution (100 mL) to give two phases. This was transferred to a pressure vessel, sealed and heated to 80° C. with stirring for 2 hours. The tetrahydrofuran was evaporated and the residue was partitioned between saturated brine and diethyl ether. The organic extracts were dried over sodium sulphate, filtered and evaporated to give a thick yellow slurry (65 gm) of crude product.

WORKUP

后处理

  1. customto give two phases
  2. customThis was transferred to a pressure vessel
  3. customsealed
  4. customThe tetrahydrofuran was evaporated
  5. customthe residue was partitioned between saturated brine and diethyl ether
  6. dry with materialThe organic extracts were dried over sodium sulphate
  7. filtrationfiltered
  8. customevaporated