反应 #44233

ord-5f3420f9dbf54f8ba647f6529ca0f879

反应方程式

CNN
methylhydrazine
CCOC(=O)C(C)=O
ethyl pyruvate
O=S(=O)([O-])[O-].[Mg+2]
MgSO4
CCOC(=O)C(C)=NNC
desired product
收率 94.0%
CCOC(=O)C(C)=NNC
ethyl 2-(2-methylhydrazono)propanoate
收率 94.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤the reaction mixture was filtered
  2. 2
    浓缩The filtrate was concentrated under reduced pressure

实验过程

To a suspension of ethyl pyruvate (37.8 mL, 338 mmol) and MgSO4 (40.8 g, 339 mmol) in CHCl3 (500 mL) was added a solution of methylhydrazine (18.0 mL, 332 mmol) in CHCl3 (100 mL) at 0° C. The reaction mixture was warmed to room temperature. After stirring for 24 hours at room temperature, the reaction mixture was filtered. The filtrate was concentrated under reduced pressure to give 44 g (94%) of the desired product that was used directly without further purification.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07732616B2uspto-grants-2010_06