HRID1830

反应详情

EQUATION

反应方程式

HRID 1830 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In concentrated hydrochloric acid (15 ml), 7-acetamido-4,10-dihydrothieno[3,2-c][1]benzoxepin-10-one obtained in Reference Example 9(0.41 g, 1.51 mmol) was heated under reflux for 2 hours. The reaction mixture was poured into a saturated aqueous solution of sodium bicarbonate, followed by extraction with ethyl acetate (25 ml). The organic layer was washed with a saturated aqueous solution of sodium chloride, and then dried over anhydrous magnesium sulfate. After the drying agent was filtered off, the organic layer was concentrated under reduced pressure to give 7-amino-4,10-dihydrothieno[3,2-c][1]benzoxepin-10-one as a yellow solid (0.28 g, 78%).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours
  3. extractionfollowed by extraction with ethyl acetate (25 ml)
  4. washThe organic layer was washed with a saturated aqueous solution of sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationAfter the drying agent was filtered off
  7. concentrationthe organic layer was concentrated under reduced pressure