HRID1594889
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
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
- concentrationThe reaction was concentrated in vacuo
- additiondiluted with MeOH (30 mL)
- temperaturerefluxed for 1 hr
- concentrationconcentrated in vacuo
- custompurified