HRID877435

反应详情

EQUATION

反应方程式

HRID 877435 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of compound 2 (2.1 g, 9.8 mmol) and hydrazine hydrate (2.4 mL, 49.0 mmol) in ethanol (70 mL) was heated to reflux for 8 h. On completion, solvent was removed, diluted with water (30 mL) and extracted with 10% methanol in dichloromethane (60 mL×4). The combined organic layer was washed with brine, dried over sodium sulphate and concentrated to afford the title compound 3 (2.0 g, 91%) which was used for further reaction.

WORKUP

后处理

  1. temperatureto reflux for 8 h
  2. customOn completion, solvent was removed
  3. additiondiluted with water (30 mL)
  4. extractionextracted with 10% methanol in dichloromethane (60 mL×4)
  5. washThe combined organic layer was washed with brine
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated