HRID1594868

反应详情

EQUATION

反应方程式

HRID 1594868 的结构方程式

PROCEDURE

实验过程

2-[3-(3-ethyl-1-methyl-2-oxo-azepan-3-yl)-phenoxy]-4-(1-trityl-1H-imidazol-4-ylmethyl)-benzonitrile (as described in Example 15, Step B) (0.074 g, 0.110 mmol) and triethylsilane (0.140 mL, 0.828 mmol) were stirred in CH2Cl2 (5 mL) and TFA (2.5 mL) for 1 h. The solution was concentrated in vacuo and purified using reverse phase chromatography (95/5-5/95 H2O/CH3CN with 0.1% TFA, flow=65 mL/min). The compound was converted to its free base using saturated NaHCO3 solution, extracted with CH2Cl2 (3×), dried (MgSO4), filtered and treated with 1N HCl ethereal solution to give the title compound.

WORKUP

后处理

  1. concentrationThe solution was concentrated in vacuo
  2. custompurified
  3. extractionextracted with CH2Cl2 (3×)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. additiontreated with 1N HCl ethereal solution