HRID1594889

反应详情

EQUATION

反应方程式

HRID 1594889 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Acetic acid (4-cyano-3-fluoro-phenyl)-(1-trityl-1H-imidazol-4-yl)-methyl ester (as described in Step C above) (4.60 g, 9.17 mmol) and dimethyl sulfate (0.83 mL, 8.81 mmol) were dissolved in EtOAc (20 mL) and heated at 60° C. overnight under Ar. The reaction was concentrated in vacuo, diluted with MeOH (30 mL), and refluxed for 1 hr, concentrated in vacuo and purified using SiO2 chromatography (0.5-4% MeOH/CH2Cl2 with NH4OH) to give the title compound.

WORKUP

后处理

  1. concentrationThe reaction was concentrated in vacuo
  2. additiondiluted with MeOH (30 mL)
  3. temperaturerefluxed for 1 hr
  4. concentrationconcentrated in vacuo
  5. custompurified