HRID1594867

反应详情

EQUATION

反应方程式

HRID 1594867 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationThe solution was concentrated in vacuo
  2. additiondiluted with EtOAc
  3. washwashed with 1N NaOH solution, water, brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated
  6. custompurified