Phosgene → 4-Benzoylbenzoyl chloride

HRID 486860

반응식

HRID 486860 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 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.

후처리

  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

출처 및 근거

ORD 기록
ord-3b637853f62e4aacababa0234e5bd8df
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292915

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