HRID1170434

反应详情

EQUATION

反应方程式

HRID 1170434 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 3-oxocyclobutane carboxylic benzyl ester (88.1 mg, 0.43 mmol) in dichloromethane (4.3 mL) were successively added diethylamine (0.18 mL, 1.73 mmol) and sodium triacetoxyborohydride (137.0 mg, 0.65 mmol). The mixture was stirred at room temperature for 5 hours, and then to the reaction solution was added saturated aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and filtered, and then evaporated. The resulting residue was purified by silica gel column chromatography (chloroform/methanol 20/1 to 5/1) to give the titled compound (66.3 mg, 59%).

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. customevaporated
  5. customThe resulting residue was purified by silica gel column chromatography (chloroform/methanol 20/1 to 5/1)