HRID1098767

反应详情

EQUATION

反应方程式

HRID 1098767 的结构方程式

PROCEDURE

实验过程

To a solution of the compound yielded from step 2 (1.20 g, 3.56 mmol) in MeOH (20 mL) ammonium acetate (2.75 g, 35.63 mmol) and sodium cyanoborohydride (224 mg, 3.56 mmol) were added. The reaction mixture was refluxed for 6 h. Then the cooled mixture was adjusted with trifluoroacetic acid to pH=2 and evaporated to dryness. Purification of the crude product by prep-HPLC and lyophilization of the relevant fractions lead to the desired product (420 mg, 26%).

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 6 h
  2. customevaporated to dryness
  3. customPurification of the crude product by prep-HPLC and lyophilization of the relevant fractions