HRID1080613

反应详情

EQUATION

反应方程式

HRID 1080613 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl cyanoformate (16.9 g, 0.171 mol) is added to a stirred solution of 5-(4-methoxyphenyl)-[1,3,4]oxathiazolin-2-one (11.9 g, 0.057 mol) in p-xylene (100 ml). The mixture is heated to 115°-132° C. for 10 hours, during which time carbon dioxide is liberated. The solvent is evaporated in vacuo and the residue is triturated with di-isopropyl ether. The crystalline solid is filtered off, washed with a small amount of diisopropyl ether and dried, to give ethyl 3-(4-methoxyphenyl)-[1,2,4]thiadiazole-5-carboxylate (11.6 g, 77%) as beige crystals, m.p. 61°-63° C.

WORKUP

后处理

  1. customThe solvent is evaporated in vacuo
  2. customthe residue is triturated with di-isopropyl ether
  3. filtrationThe crystalline solid is filtered off
  4. washwashed with a small amount of diisopropyl ether
  5. customdried