Oxalyl chloride → 2,6-Difluorobenzoyl isocyanate
反応式
C(Cl)(=O)[C:2](Cl)=[O:3].[F:7][C:8]1[CH:16]=[CH:15][CH:14]=[C:13]([F:17])[C:9]=1[C:10]([NH2:12])=[O:11]>ClCCCl>[F:7][C:8]1[CH:16]=[CH:15][CH:14]=[C:13]([F:17])[C:9]=1[C:10]([N:12]=[C:2]=[O:3])=[O:11]参加物
4
実験手順
Oxalyl chloride (5.5 g) was added slowly to a suspension of 2,6-difluorobenzamide (6.0 g) in 1,2-dichloroethane maintained at a temperature within the range -10° to -5° C. When the addition was complete the mixture was allowed to warm to the ambient temperature, and then gradually heated to the reflux temperature and maintained thereat for a period of 16 hours. The solvent was then removed by evaporation under reduced pressure and the residual oil purified by distillation to yield 2,6-difluorobenzoyl isocyanate, b.p. 60°-61°/0.7 mm.
後処理
- temperaturemaintained at a temperature within the range -10° to -5° C
- additionWhen the addition
- temperaturegradually heated to the reflux temperature
- temperaturemaintained
- customThe solvent was then removed by evaporation under reduced pressure
- distillationthe residual oil purified by distillation
出典と根拠
- ORDレコード
- ord-f779bab063b2461595cd6647fbefa252
- 出典データセット
- uspto-grants-1979_04
- 特許番号
- US04150158
反応ノート
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