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Thionyl Chloride → 4-(Chlorocarbonyl)phenyl benzoate

HRID 854223
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HRID 854223 반응식
[C:1]([O:9][C:10]1[CH:18]=[CH:17][C:13]([C:14](O)=[O:15])=[CH:12][CH:11]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(Cl)([Cl:21])=O>CN(C)C=O>[C:1]([O:9][C:10]1[CH:18]=[CH:17][C:13]([C:14]([Cl:21])=[O:15])=[CH:12][CH:11]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 119979Benzoic acid, 4-(benzoyloxy)-

생성물 1

HCID 150272094-(Chlorocarbonyl)phenyl benzoate

시약·촉매·용매 1

HCID 6228Dimethylformamide촉매

실험 절차

10.00 g (41.3 mmol) of 4-(benzoyloxy)benzoic acid and one drop of N,N-dimethylformamide are refluxed in 40 ml of thionyl chloride with stirring until gas is no longer evolved. The excess thionyl chloride is very substantially removed by distillation under reduced pressure and co-distilled twice with petroleum ether (50/70) under reduced pressure from the remaining residue for complete removal. Purification is carried out by recrystallization from 150 ml of petroleum ether (50/70)/ethyl acetate 2:1, and the crystals are washed with 4 ml of petroleum ether (50/70)

후처리

  1. customThe excess thionyl chloride is very substantially removed by distillation under reduced pressure
  2. customco-distilled twice with petroleum ether (50/70) under reduced pressure from the remaining residue for complete removal
  3. customPurification
  4. customis carried out by recrystallization from 150 ml of petroleum ether (50/70)/ethyl acetate 2:1
  5. washthe crystals are washed with 4 ml of petroleum ether (50/70)

출처 및 근거

ORD 기록
ord-c5bb76b319364229ad4cf68f04c53584
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07258902B2

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