HRID1426372

反应详情

EQUATION

反应方程式

HRID 1426372 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-[M ethyl-(5-trifluoromethyl-[1,3,4]thiadiazol-2-yl)-amino]-piperidine-1-carboxylic acid benzyl ester (D1) (0.91 g, 2.27 mmol) in a solution 6 N of hydrochloric acid (15 ml) was stirred at 150° C. for 10 min., under microwave irradiation. After cooling to room temperature, the reaction mixture was diluted with water and extracted with dichloromethane (25 ml). The aqueous layer was basified with a saturated solution of sodium carbonate and extracted with dichloromethane (3×25 ml). The combined organic extracts were dried (Na2SO4) and the solvent evaporated in vacuo to yield D2 (0.56 g, 93%) as a solid. C9H13F3N4S requires 266. Found 266 (MH+).

WORKUP

后处理

  1. extractionextracted with dichloromethane (25 ml)
  2. extractionextracted with dichloromethane (3×25 ml)
  3. dry with materialThe combined organic extracts were dried (Na2SO4)
  4. customthe solvent evaporated in vacuo