HRID889238

反应详情

EQUATION

反应方程式

HRID 889238 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of imidazole (4.5 g, 66.6 mmol) and PPh3 (17.4 g, 66.6 mmol) in DCM (180 mL) is slowly added over a period of 10 min of I2 (16.9 g, 66.6 mmol) and it is stirred at RT for 30 min. Then a solution of methanesulfonic acid 2-hydroxymethyl-5-methylphenyl ester (12.0 g, 55.5 mmol) in DCM (40 mL) is added drop wise and it is stirred at RT for 1 h. The reaction mixture is concentrated to about 70 mL. It is then filtered and washed with DCM. The filtrate is concentrated and purified to give the title compound as a solid.

WORKUP

后处理

  1. stirringit is stirred at RT for 1 h
  2. concentrationThe reaction mixture is concentrated to about 70 mL
  3. filtrationIt is then filtered
  4. washwashed with DCM
  5. concentrationThe filtrate is concentrated
  6. custompurified