HRID1422616

反应详情

EQUATION

反应方程式

HRID 1422616 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-methyl-4,5,6,7-tetrahydro-thiazolo[5,4-c]pyridine (3.00 g), potassium bromomethyltrifluoroborate (3.91 g), KHCO3 (1.95 g), KI (0.32 g), and tetrahydrofuran (25 mL) is stirred at reflux temperature for 4 h. After cooling to room temperature, the solvent is evaporated and the residue is suspended in acetone. The insoluble salts are separated by filtration and the filtrate is treated with diethyl ether. The precipitate is separated by filtration and dried to give the title compound (alternatively, the crude product is purified by chromatography on silica gel using dichloromethane and methanol as eluent). Mass spectrum (ESI−): m/z=235 [M]−.

WORKUP

后处理

  1. temperatureat reflux temperature for 4 h
  2. customthe solvent is evaporated
  3. customThe insoluble salts are separated by filtration
  4. additionthe filtrate is treated with diethyl ether
  5. customThe precipitate is separated by filtration
  6. customdried