HRID1979042

反应详情

EQUATION

反应方程式

HRID 1979042 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of the above ester (0.6 g, 0.0015 mol) in ethanol (5 ml) 4 N sodium hydroxide (0.8 ml) was added and the mixture was stirred at room temperature for 2.5 h and then left in a freezer overnight. The cold reaction mixture was allowed to warm to room temperature during 1 h, and 4 N hydrochloric acid (1.2 ml) and water (10 ml) were added. The mixture was extracted with dichloromethane (2×100 ml). The combined organic extracts were dried (MgSO4) and the solvent was evaporated in vacuo. The residue was reevaporated with a mixture of acetone and isopropyl acetate and then treated with a mixture of acetone and isopropyl acetate to give a solid which was isolated and dried in vacuo. This afforded 0.33 g of the title compound.

WORKUP

后处理

  1. waitleft in a freezer overnight
  2. customThe cold reaction mixture
  3. temperatureto warm to room temperature during 1 h
  4. extractionThe mixture was extracted with dichloromethane (2×100 ml)
  5. dry with materialThe combined organic extracts were dried (MgSO4)
  6. customthe solvent was evaporated in vacuo
  7. customThe residue was reevaporated with a mixture of acetone and isopropyl acetate
  8. additiontreated with a mixture of acetone and isopropyl acetate
  9. customto give a solid which
  10. customwas isolated
  11. customdried in vacuo