HRID68937

反应详情

EQUATION

反应方程式

HRID 68937 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
145 °C

PROCEDURE

实验过程

The mixture of 5-(5-trifluoromethyl-pyridin-2-yl)-4,5,6,7-tetrahydro-thiazolo[5,4-c]pyridin-2-ylamine (5.7 gm, 0.019 mol) and triethyl methantricarboxylate (16.1 ml, 0.076 mol) in xylene (100 ml) was heated at 140-150° C. for 6 hours. Xylene was evaporated and diethyl ether was then added and the suspension was stirred for 15 minutes. It was filtered and washed with ether. The crude solid was digested with dichloromethane (200 ml) and filtered to remove insoluble residue. Dichloromethane layer was distilled off under vacuum to give 1.3 gm of title compound.

WORKUP

后处理

  1. customXylene was evaporated
  2. additiondiethyl ether was then added
  3. filtrationIt was filtered
  4. washwashed with ether
  5. filtrationfiltered
  6. customto remove insoluble residue
  7. distillationDichloromethane layer was distilled off under vacuum