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

HRID 44197노트

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HRID 44197 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 mot) 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-bc1df6958e8c495a952b555eab578d2a
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541410B2

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