HRID1446652

反应详情

EQUATION

反应方程式

HRID 1446652 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 4,4-dimethyl-3-oxo-pentanenitrile (5.0 g, 0.04 mol) in absolute ethanol (50 mL), add 2-hydrazino-ethanol (3 mL, 1.1 equiv.) and concentrated HCl (0.5 mL). Reflux the reaction for 4 hours then cool to room temperature and dilute with water and ethyl acetate. Wash the organics with water then saturated aqueous saturated sodium chloride then dry with magnesium sulfate, filter and concentrate in vacuo. Trituration from hexanes and dichloromethane gives a white solid (4.8 g, 66%). MS (ES), m/z 184 (M+1).

WORKUP

后处理

  1. temperatureReflux
  2. customthe reaction for 4 hours
  3. washWash the organics with water
  4. dry with materialsaturated aqueous saturated sodium chloride then dry with magnesium sulfate
  5. filtrationfilter
  6. concentrationconcentrate in vacuo