HRID1098743
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 from step 1 (630 mg, 1.79 mmol) in MeOH (30 mL) ammonium acetate (1.39 g, 17.9 mmol) was added. After stirring at ambient temperature overnight sodium cyanoborohydride (135.7 mg, 2.16 mmol) was added and the reaction was refluxed for 6 h. The solvent was evaporated and the solid, dissolved in ethyl acetate, was extracted with water. The organic layer was separated, washed with brine, dried over sodium sulphate, filtered and evaporated to give 606 mg (yield: 96%) of the crude product. LC/MS (method D) (M+H)+: 352
WORKUP
后处理
- additionwas added
- temperaturethe reaction was refluxed for 6 h
- customThe solvent was evaporated
- dissolutionthe solid, dissolved in ethyl acetate
- extractionwas extracted with water
- customThe organic layer was separated
- washwashed with brine
- dry with materialdried over sodium sulphate
- filtrationfiltered
- customevaporated