Oxalyl chloride → 2,6-Difluorobenzoyl isocyanate

HRID 26536

반응식

HRID 26536 반응식
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]

참가 물질

4

반응물 2

HCID 65578Oxalyl chlorideHCID 874392,6-Difluorobenzamide

생성물 1

HCID 27333692,6-Difluorobenzoyl isocyanate

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

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.

후처리

  1. temperaturemaintained at a temperature within the range -10° to -5° C
  2. additionWhen the addition
  3. temperaturegradually heated to the reflux temperature
  4. temperaturemaintained
  5. customThe solvent was then removed by evaporation under reduced pressure
  6. distillationthe residual oil purified by distillation

출처 및 근거

ORD 기록
ord-f779bab063b2461595cd6647fbefa252
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04150158

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