反応 #944

ord-57d496f8cfa74e14b0b60ed9b08a5969

反応方程式

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

溶媒

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  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
    ろ過The suspension was filtered
  9. 9
    その他the solid product dried

実験手順

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.

出典

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