Phosgene → 4-Benzoylbenzoyl chloride

HRID 6453

반응식

HRID 6453 반응식
[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]

참가 물질

5

반응물 2

HCID 6371Phosgene3회HCID 143474-Hydroxybenzophenone

생성물 1

HCID 129121414-Benzoylbenzoyl chloride수율 99.2%

시약·촉매·용매 2

HCID 5963Benzyltrimethylammonium chloride촉매HCID 7237O-Xylene용매

실험 절차

A total of 3.4 kg of phosgene were passed in the course of 5 hours into a solution of 4 kg of 4-hydroxybenzophenone and 190 g of benzyltrimethylammonium chloride in 11.4 kg of o-xylene. During this time, the internal temperature was increased from 95° to 1200° C. After the end of the introduction of phosgene, stirring was continued for 30 minutes at 115° C. Working up was carried out by expelling the excess phosgene with nitrogen. The salt (catalyst) precipitated toward the end of the reaction was filtered off and the solvent was distilled off. 4.9 kg (93%) of yellowish 4-chloroformylbenzophenone of melting point 67°-72° C. were obtained. This crude product containing 12.69% of Cl- (theoretical value 13.60%) was used directly for the subsequent reactions, without further purification.

후처리

  1. temperatureDuring this time, the internal temperature was increased from 95° to 1200° C
  2. customThe salt (catalyst) precipitated toward the end of the reaction
  3. filtrationwas filtered off
  4. distillationthe solvent was distilled off

출처 및 근거

ORD 기록
ord-a09f60cece474e8a9b8d9edbc056d2df
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05248805

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