HRID1080613
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
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
- customThe solvent is evaporated in vacuo
- customthe residue is triturated with di-isopropyl ether
- filtrationThe crystalline solid is filtered off
- washwashed with a small amount of diisopropyl ether
- customdried