Phosgene → 4-Bromo-2-fluoro-1-(isocyanatomethyl)benzene

HRID 726841

반응식

HRID 726841 반응식
[C:1](Cl)(Cl)=[O:2].[Br:5][C:6]1[CH:13]=[CH:12][C:9]([CH2:10][NH2:11])=[C:8]([F:14])[CH:7]=1>ClC1C=CC=CC=1>[Br:5][C:6]1[CH:13]=[CH:12][C:9]([CH2:10][N:11]=[C:1]=[O:2])=[C:8]([F:14])[CH:7]=1

참가 물질

4

반응물 2

HCID 6371Phosgene2회HCID 3770848(4-Bromo-2-fluorophenyl)methanamine

생성물 1

HCID 158174014-Bromo-2-fluoro-1-(isocyanatomethyl)benzene수율 69.1%

시약·촉매·용매 1

HCID 7964Chlorobenzene용매2회

실험 절차

Chlorobenzene (30 ml) is introduced into the reaction vessel at 60° C. and saturated with phosgene. A solution of 4-bromo-2-fluorobenzylamine (20.4 g, 0.10 mol) in chlorobenzene (40 ml) is added dropwise at 60° C. over 3 hours. At the same time, phosgene is passed in. Stirring of the batch is continued for 2 hours at 60° C., and the mixture is subsequently refluxed to remove the gases phosgene and hydrogen chloride. The batch is worked up by distillation. 15.9 g of 4-bromo-2-fluorobenzyl isocyanate (boiling point 109° C. at 4 mbar) are obtained. Yield: 69.1% of theory.

후처리

  1. temperaturethe mixture is subsequently refluxed
  2. customto remove the gases phosgene and hydrogen chloride
  3. distillationThe batch is worked up by distillation

출처 및 근거

ORD 기록
ord-ba985a8a15ca421ab9dee434a34c716e
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05710319

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