HRID2088096

反应详情

EQUATION

反应方程式

HRID 2088096 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (1R*,2R*,5S*,6R*)-8-benzyl-1-phenyl-6-phenylsulphonyl-8-azabicyclo[3.2.1]octan-2-ol (Description 4; 0.98 g, 2.25 mmol), triethylamine (0.6 ml), N,N-dimethylaminopyridine (100 mg) and 3,5-bis(trifluoromethyl)benzoyl chloride (0.6 ml, 3.33 mmol) in dry dichloromethane (10 ml) was stirred at room temperature for 6 days. The reaction mixture treated with saturated aqueous NaHCO3 and extracted with dichloromethane. The combined organic extracts were dried (Na2SO4) and concentrated. The residue was purified by chromatography on silica gel (iso-hexane:ethyl acetate 5-30%) to give the title compound (1.05 g, 69%).

WORKUP

后处理

  1. extractionextracted with dichloromethane
  2. dry with materialThe combined organic extracts were dried (Na2SO4)
  3. concentrationconcentrated
  4. customThe residue was purified by chromatography on silica gel (iso-hexane:ethyl acetate 5-30%)