HRID617165
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In 20 ml of ethanol was dissolved 2.10 g (3.32 mmol) of Compound 54 obtained in Example 54, excess sodium borohydride was added, and the mixture was stirred under heating at reflux for 1 hour. After cooling, the solvent was removed, water was added and the mixture was subjected to extraction with ethyl acetate. The organic layer was washed with sodium chloride solution, dried and concentrated to give residue. The residue was purified by silica gel column chromatography(eluent: chloroform/methanol=100/1) and recrystallized from ethanol to give 1.29 g (yield: 66%) of Compound 55 as white crystals.
WORKUP
后处理
- additionwas added
- temperatureunder heating
- temperatureat reflux for 1 hour
- temperatureAfter cooling
- customthe solvent was removed
- additionwater was added
- extractionthe mixture was subjected to extraction with ethyl acetate
- washThe organic layer was washed with sodium chloride solution
- customdried
- concentrationconcentrated
- customto give residue
- customThe residue was purified by silica gel column chromatography(eluent
- customchloroform/methanol=100/1) and recrystallized from ethanol