反应 #944

ord-57d496f8cfa74e14b0b60ed9b08a5969

反应方程式

CCC(N)C(=O)O
2-aminobutyric acid
O=S(Cl)Cl
thionyl chloride
CCOCC
diethyl ether
CCOC(=O)C(N)CC.Cl
desired product
CCOC(=O)C(N)CC.Cl
Ethyl 2-aminobutyrate hydrochloride

溶剂

反应条件

温度
0°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度gradually warmed to room temperature
  2. 2
    温度The resulting white slurry was heated
  3. 3
    温度under reflux for 3 hours
  4. 4
    workup.WAITleft
  5. 5
    温度to cool for 10 minutes
  6. 6
    workup.ADDITIONpoured
  7. 7
    workup.STIRRINGwith hand stirring
  8. 8
    过滤The suspension was filtered
  9. 9
    其他the solid product dried

实验过程

A slurry of 2-aminobutyric acid (100 g, Aldrich) in absolute ethanol (300 ml) was stirred under nitrogen at 0° C. and thionyl chloride (120.8 g) was added dropwise. The reaction was stirred overnight at 0° C. and then gradually warmed to room temperature. The resulting white slurry was heated under reflux for 3 hours, left to cool for 10 minutes, then poured into chilled diethyl ether (600 ml), with hand stirring. The suspension was filtered and the solid product dried to give the desired product (150 g) as a white solid. 1H NMR consistent with proposed structure.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05723458uspto-grants-1998_03