HRID1402349

反应详情

EQUATION

反应方程式

HRID 1402349 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Hydrazino-ethanol (2.98 mL, 44.0 mmol) was added to a stirred solution of 4,4-dimethyl-3-oxo-pentanenitrile (5.0 g, 40.0 mmol) in EtOH (IMS grade, 40 mL) at RT followed by concentrated HCl (0.4 mL). The reaction mixture was heated at reflux temperature for 18 h then cooled and concentrated in vacuo. The resultant residue was triturated with pentane to give the title compound (7.4 g, quantitative) as a yellow solid. LCMS (Method 3): Rt 0.81 min, m/z 184 [MH+].

WORKUP

后处理

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux temperature for 18 h
  3. temperaturethen cooled
  4. concentrationconcentrated in vacuo
  5. customThe resultant residue was triturated with pentane