反応 #4527

ord-a75633828b0a48b69e9a6ab1c8a89eba

反応方程式

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

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooled in a water bath
  2. 2
    洗浄The organic phase is washed with 2×50 ml of water
  3. 3
    乾燥dried over magnesium sulphate
  4. 4
    その他After evaporation and distillation, 38.1 g (73%) of α-chloroethoxycarbonylimidazole [B.p. 80° C./66.6 Pa (0.5 mm Hg)]
  5. 5
    その他are obtained in the form of a colourless liquid which
  6. 6
    その他crystallises spontaneously at room temperature

実験手順

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##

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04725680uspto-grants-1988_02