HRID1525218
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 solution of compound 4-f in HCl/dioxane (100 ml) was stirred at room temperature overnight. The mixture was then concentrated under vacuum and the residue was diluted with water followed by extraction with ethyl acetate. The aqueous layer was basified with ammonia and then extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate and concentrated to provide the product, 4-g, (1.5 g, 58%). 1H NMR (CD3OD, 300 MHz,): δ 8.64 (s, 1H), 7.77 (m, 2H), 7.22 (m, 5H), 5.16 (s, 1H), 4.07 (m, 4H), 1.22 (m, 6H). (M+H)+=321.
WORKUP
后处理
- concentrationThe mixture was then concentrated under vacuum
- additionthe residue was diluted with water
- extractionfollowed by extraction with ethyl acetate
- extractionextracted with ethyl acetate
- washThe organic layer was washed with brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated