HRID1098767
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureThe reaction mixture was refluxed for 6 h
- customevaporated to dryness
- customPurification of the crude product by prep-HPLC and lyophilization of the relevant fractions