Oxalyl chloride → 2,6-Difluorobenzoyl isocyanate

HRID 26536

反応式

HRID 26536 の反応式
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

反応物 2

HCID 65578Oxalyl chlorideHCID 874392,6-Difluorobenzamide

生成物 1

HCID 27333692,6-Difluorobenzoyl isocyanate

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

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

  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

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

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