Phosgene → 4-Bromo-2-fluoro-1-(isocyanatomethyl)benzene
反応式
[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]=1参加物
4
実験手順
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.
後処理
- temperaturethe mixture is subsequently refluxed
- customto remove the gases phosgene and hydrogen chloride
- distillationThe batch is worked up by distillation
出典と根拠
- ORDレコード
- ord-ba985a8a15ca421ab9dee434a34c716e
- 出典データセット
- uspto-grants-1998_01
- 特許番号
- US05710319
反応ノート
読み込み中…