HRID2371641
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
A mixture of 150 mg (0.277 mmol) of the titled product of Example 60, 3 ml of methanol, and 3 ml of 1N sodium hydroxide was stirred at reflux for one hour. The reaction mixture was permitted to cool and then partitioned between ethyl acetate and 3N hydrochloric acid. The aqueous layer was further extracted with two portions of ethyl acetate. The combined organic extracts were washed with brine, dried (MgSO4), filtered, and the solvent removed under reduced pressure. Crystallization of the residue from ethyl acetate gave 24 mg of the title compound as a solid, m.p. 159.5°-161.5° C.
WORKUP
后处理
- temperatureat reflux for one hour
- temperatureto cool
- custompartitioned between ethyl acetate and 3N hydrochloric acid
- extractionThe aqueous layer was further extracted with two portions of ethyl acetate
- washThe combined organic extracts were washed with brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- customthe solvent removed under reduced pressure
- customCrystallization of the residue from ethyl acetate