Phosphorus pentachloride → 2-(4-Chloro-phenylsulfonylamino)4,5-dimethoxy-benzoyl chloride

HRID 425749노트

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HRID 425749 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:20]=[C:19]([O:21][CH3:22])[C:18]([O:23][CH3:24])=[CH:17][C:13]=2[C:14](O)=[O:15])(=[O:10])=[O:9])=[CH:4][CH:3]=1.P(Cl)(Cl)(Cl)(Cl)[Cl:26]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12]2[CH:20]=[C:19]([O:21][CH3:22])[C:18]([O:23][CH3:24])=[CH:17][C:13]=2[C:14]([Cl:26])=[O:15])(=[O:10])=[O:9])=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 24819Phosphorus pentachlorideHCID 12399912-{[(4-Chlorophenyl)sulfonyl]amino}-4,5-dimethoxybenzoic acid

생성물 1

HCID 98433672-(4-Chloro-phenylsulfonylamino)4,5-dimethoxy-benzoyl chloride수율 93%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
42.5 °C

실험 절차

25.90 g (0.07 mol) of 2-(4-chloro-phenylsulfonylamino)-4,5-dimethoxy-benzoic acid were mixed with 75 ml of toluene, 17.30 g (0.08 mol) of phosphorus pentachloride were added and the mixture was stirred at 40-45° C. for 2.5 h. Then the mixture was concentrated in vacuo to half of its volume and the product that precipitated was filtered off with suction and washed with a small amount of toluene. 25.30 g (93%) of 2-(4-chloro-phenylsulfonylamino)-4,5-dimethoxy-benzoyl chloride having a melting point of 175-177° C. were obtained.

후처리

  1. additionwere added
  2. concentrationThen the mixture was concentrated in vacuo to half of its volume
  3. customthe product that precipitated
  4. filtrationwas filtered off with suction
  5. washwashed with a small amount of toluene

출처 및 근거

ORD 기록
ord-17f0651b37a440758c4ad635bf1ae911
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08106213B2

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