Water → 2,3-Dichloro-6-(trifluoromethyl)benzonitrile

HRID 1005482ノート

反応式

HRID 1005482 の反応式
[Cl:1][C:2]1[C:10]([Cl:11])=[CH:9][CH:8]=[C:7]([C:12]([F:15])([F:14])[F:13])[C:3]=1[C:4]([NH2:6])=O.P(Cl)(Cl)(Cl)=O.O>C1C=CC=CC=1>[Cl:1][C:2]1[C:10]([Cl:11])=[CH:9][CH:8]=[C:7]([C:12]([F:15])([F:13])[F:14])[C:3]=1[C:4]#[N:6]

参加物

5

反応物 3

HCID 962WaterHCID 24813Phosphorus oxychloride2 回HCID 154569832,3-Dichloro-6-(trifluoromethyl)benzamide

生成物 1

HCID 109775462,3-Dichloro-6-(trifluoromethyl)benzonitrile収率 95.8%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

反応条件

温度
35 °C

実験手順

To a solution of 229 g of 2,3-dichloro-6-trifluoromethylbenzamide in 2 liters of benzene was added 409 g of phosphorus oxychloride and then the mixture was heated at ref lux for 3.5 hours. After cooling, the solution was gradually added into 2 liters of water maintained at 30-40° C. to hydrolyze the excess phosphorus oxychloride therein and was allowed to separation. The aqueous layer was extracted with benzene, and the extract was combined with the organic layer previously obtained, washed with water and with saturated saline solution and dried over anhydrous magnesium sulfate. The solvent was distilled under reduced pressure, and the crude product obtained was washed with n-hexane and filtered to obtain 204 g of the title compound(mp. 53-54° C.).

後処理

  1. temperaturethe mixture was heated at ref lux for 3.5 hours
  2. temperatureAfter cooling
  3. customwas allowed to separation
  4. extractionThe aqueous layer was extracted with benzene
  5. custompreviously obtained
  6. washwashed with water and with saturated saline solution
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationThe solvent was distilled under reduced pressure
  9. customthe crude product obtained
  10. washwas washed with n-hexane
  11. filtrationfiltered

出典と根拠

ORDレコード
ord-bf5c0b36694746b98409c37ab334a751
出典データセット
uspto-grants-2000_04
特許番号
US06054605

反応ノート

読み込み中…