HRID1434617

反应详情

EQUATION

反应方程式

HRID 1434617 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of hydrazine hydrate (10 ml) in ethanol (100 ml) at 0° C. was added a solution of (benzyloxy)acetyl chloride (6.4 ml) in THF (40 ml) by syringe pump over 30 minutes. The reaction mixture was allowed to warm to room temperature and stirred for 18 hours. The ethanol was removed under reduced pressure and the remaining aqueous mixture extracted with dichloromethane (3×100 ml). The combined organic extracts were washed with aqueous K2CO3 (100 ml) then brine (100 ml) and dried (MgSO4). Concentration under reduced pressure gave 2-(benzyloxy)acetohydrazide as a colourless oil that crystallized on standing (5.5 g).

WORKUP

后处理

  1. customThe ethanol was removed under reduced pressure
  2. extractionthe remaining aqueous mixture extracted with dichloromethane (3×100 ml)
  3. washThe combined organic extracts were washed with aqueous K2CO3 (100 ml)
  4. dry with materialbrine (100 ml) and dried (MgSO4)
  5. concentrationConcentration under reduced pressure