HRID1594867
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
PROCEDURE
实验过程
2-Fluoro-4-(1-trityl-1H-imidazol-4-ylmethyl)-benzonitrile (as described in Step A above) (0.348 g, 0.784 mmol), 3-ethyl-3-(3-hydroxy-phenyl)-1-methyl-azepan-2-one (as described in Example 8, Step B) (0.194 mg, 0.784 mmol), KF.Al2O3 (0.232 g) and 18-Crown-6 (0.020 g, 0.076 mmol) were refluxed in CH3CN (15 mL) under Ar for 48 h. The solution was concentrated in vacuo, diluted with EtOAc, washed with 1N NaOH solution, water, brine, dried (MgSO4), concentrated and purified using SiO2 chromatography (1.0% MeOH/CH2Cl2) to give the title compound.
WORKUP
后处理
- concentrationThe solution was concentrated in vacuo
- additiondiluted with EtOAc
- washwashed with 1N NaOH solution, water, brine
- dry with materialdried (MgSO4)
- concentrationconcentrated
- custompurified