HRID2047477
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
To a solution of the compound (5.2 g) obtained in step 1 in THF/methanol/water (6.0/18/9.5 mL) was added 4N aqueous lithium hydroxide solution (9.5 mL), and the mixture was stirred at room temperature for 4 hr. The mixture was acidified with 1N hydrochloric acid, concentrated under reduced pressure, diluted with water, and extracted with ethyl acetate. The extract was washed with water and saturated brine, dried, filtered through silica gel (eluted with ethyl acetate). The filtrate was concentrated under reduced pressure, and crystallized from ethyl acetate/hexane to give the title compound (4.3 g, 86%) as a pale-yellow powder.
WORKUP
后处理
- concentrationconcentrated under reduced pressure
- additiondiluted with water
- extractionextracted with ethyl acetate
- washThe extract was washed with water and saturated brine
- customdried
- filtrationfiltered through silica gel (eluted with ethyl acetate)
- concentrationThe filtrate was concentrated under reduced pressure
- customcrystallized from ethyl acetate/hexane