반응 #215068

ord-bef6bd1d7fd2460e9a65c80d4826ceec

반응 방정식

CC(=O)C(=O)O
pyruvic acid
O=C(Cl)OCC(Cl)(Cl)Cl
trichloroethyl chloroformate
c1ccncc1
pyridine
CC(=O)C(=O)OCC(Cl)(Cl)Cl
trichloroethyl pyruvate
수율 50.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축the mixture is concentrated in vacuum
  2. 2
    workup.ADDITIONdiluted with water
  3. 3
    추출extracted with ethyl acetate
  4. 4
    세척The extract is washed with 5% HCl
  5. 5
    건조dried over MgSO4
  6. 6
    기타evaporated
  7. 7
    workup.DISTILLATIONdistilled in vacuum

실험 절차

To a solution of 3.3 g (37.5 mmole) of pyruvic acid and 7.9 g (37.5 mmole) of trichloroethyl chloroformate in 20 ml of dry tetrahydrofuran at 0° is added dropwise 0.6 ml of pyridine. After stirring for 2 hours at room temperature, the mixture is concentrated in vacuum, diluted with water and extracted with ethyl acetate. The extract is washed with 5% HCl, dried over MgSO4, evaporated and distilled in vacuum to give 4.0 g (50%) trichloroethyl pyruvate, bp 75°-82° (17 mm).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04257947uspto-grants-1981_03