光气 → 4-苯甲酰基苯甲酰氯

HRID 6453

反应方程式

HRID 6453 反应方程式
[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]

参与物

5

反应物 2

HCID 6371光气3 次HCID 143474-羟基-二苯甲酮

产物 1

HCID 129121414-苯甲酰基苯甲酰氯收率 99.2%

试剂、催化剂与溶剂 2

HCID 5963苄基三甲基氯化铵催化剂HCID 7237邻二甲苯溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-a09f60cece474e8a9b8d9edbc056d2df
来源数据集
uspto-grants-1993_09
专利号
US05248805

关联笔记

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