반응 #944

ord-57d496f8cfa74e14b0b60ed9b08a5969

반응 방정식

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

용매

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도gradually warmed to room temperature
  2. 2
    온도The resulting white slurry was heated
  3. 3
    온도under reflux for 3 hours
  4. 4
    workup.WAITleft
  5. 5
    온도to cool for 10 minutes
  6. 6
    workup.ADDITIONpoured
  7. 7
    workup.STIRRINGwith hand stirring
  8. 8
    여과The suspension was filtered
  9. 9
    기타the solid product dried

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05723458uspto-grants-1998_03