HRID1525218

反应详情

EQUATION

反应方程式

HRID 1525218 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationThe mixture was then concentrated under vacuum
  2. additionthe residue was diluted with water
  3. extractionfollowed by extraction with ethyl acetate
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated