Phosgene → 4-Benzoylbenzoyl chloride

HRID 486860

反応式

HRID 486860 の反応式
[C:1]([Cl:4])(Cl)=[O:2].O[C:6]1[CH:19]=[CH:18][C:9]([C:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[O:11])=[CH:8][CH:7]=1>[Cl-].C([N+](C)(C)C)C1C=CC=CC=1.CC1C=CC=CC=1C>[Cl:4][C:1]([C:15]1[CH:16]=[CH:17][C:12]([C:10]([C:9]2[CH:18]=[CH:19][CH:6]=[CH:7][CH:8]=2)=[O:11])=[CH:13][CH:14]=1)=[O:2]

参加物

5

反応物 2

HCID 6371Phosgene3 回HCID 143474-Hydroxybenzophenone

生成物 1

HCID 129121414-Benzoylbenzoyl chloride収率 99.2%

試薬・触媒・溶媒 2

HCID 5963Benzyltrimethylammonium chloride触媒HCID 7237O-Xylene溶媒

実験手順

A total of 3.4 kg of phosgene was passed through a solution of 4 kg of 4-hydroxybenzophenone and 190 g of benzyltrimethylammonium chloride in 11.4 kg of o-xylene over a period of 5 hours, during which time the internal temperature was raised from 95° to 120° C. The introduction of phosgene was then stopped, and stirring was continued for 30 minutes at 115° C. Before the product was worked up, the excess phosgene was expelled with nitrogen. The salt (catalyst) which precipitated toward the end of the reaction was filtered off, and the solvent was removed by distillation. There were obtained 4.9 kg (93%) of yellowish 4-chloroformylbenzophenone having a melting point of 67°-72° C. This crude product having a Cl content of 12.69% (theory=13.60%) was used unpurified as starting material for subsequent reactions.

後処理

  1. temperaturethe internal temperature was raised from 95° to 120° C
  2. customThe salt (catalyst) which precipitated toward the end of the reaction
  3. filtrationwas filtered off
  4. customthe solvent was removed by distillation

出典と根拠

ORDレコード
ord-3b637853f62e4aacababa0234e5bd8df
出典データセット
uspto-grants-1994_03
特許番号
US05292915

関連ノート

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