반응 #4527

ord-a75633828b0a48b69e9a6ab1c8a89eba

반응 방정식

O=C(Cl)OCCCl
chloroethyl chloroformate
c1c[nH]cn1
imidazole
ClCCl
dichloromethane
O
water
CC(Cl)OC(=O)c1ncc[nH]1
α-chloroethoxycarbonylimidazole

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooled in a water bath
  2. 2
    세척The organic phase is washed with 2×50 ml of water
  3. 3
    건조dried over magnesium sulphate
  4. 4
    기타After evaporation and distillation, 38.1 g (73%) of α-chloroethoxycarbonylimidazole [B.p. 80° C./66.6 Pa (0.5 mm Hg)]
  5. 5
    기타are obtained in the form of a colourless liquid which
  6. 6
    기타crystallises spontaneously at room temperature

실험 절차

28.6 g (0.2 mole) of chloroethyl chloroformate are added dropwise to a solution of 27.2 g (0.4 mole) of imidazole in 200 ml of dichloromethane cooled in a water bath. The mixture is stirred at room temperature for 4 hours, and 50 ml of iced water are then added. The organic phase is washed with 2×50 ml of water and then dried over magnesium sulphate. After evaporation and distillation, 38.1 g (73%) of α-chloroethoxycarbonylimidazole [B.p. 80° C./66.6 Pa (0.5 mm Hg)] are obtained in the form of a colourless liquid which crystallises spontaneously at room temperature, m.p. 50° C. ##STR57##

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04725680uspto-grants-1988_02