HRID8754

反应详情

EQUATION

反应方程式

HRID 8754 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 tert-butyl 2-(methoxycarbonyl)-1-oxo-8-azaspiro[4.5]decane-8-carboxate from Procedure 1, Step F (0.448 g, 1.46 mmol) in toluene (15 mL) was added hydrazine (0.084 mL, 1.72 mmol). The reaction mixture was refluxed for 12 h, concentrated and the residue was purified by flash chromatography eluting with 5% MeOH/dichloromethane and 0.1% triethylamine to give the title compound (0.263 g). MS/EI (acetonitrile/water): m/z 294.3 retention time=2.0 min.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 12 h
  2. concentrationconcentrated
  3. customthe residue was purified by flash chromatography
  4. washeluting with 5% MeOH/dichloromethane and 0.1% triethylamine