Pyridine → HCID 53972694, 화합물

HRID 248750

반응식

HRID 248750 반응식
[F:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([C:9]([F:12])([F:11])[F:10])[CH:3]=1.N1C=CC=CC=1.[CH3:19][O:20][C:21](=[O:32])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[S:28](Cl)(=[O:30])=[O:29]>ClCCl>[CH3:19][O:20][C:21](=[O:32])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][C:23]=1[S:28](=[O:29])(=[O:30])[NH:6][C:5]1[CH:7]=[CH:8][C:2]([F:1])=[CH:3][C:4]=1[C:9]([F:10])([F:11])[F:12]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 678534-Fluoro-2-(trifluoromethyl)anilineHCID 117830Benzoic acid, 2-(chlorosulfonyl)-, methyl ester

생성물 1

HCID 53972694HCID 53972694, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

250 ml of dichloromethane is combined with 9.38 g (52.37 mmol) of 4-fluoro-2-trifluoromethylaniline and 6 ml (14.3 mmol) of pyridine. The mixture is cooled with ice water and under agitation and exclusion of moisture, 13.52 g (57.62 mmol) of 2-chlorosulfonylbenzoic acid methyl ester is added in small increments. The mixture is agitated overnight, washed with 2N hydrochloric acid and water, the dichloromethane solution is dried over sodium sulfate and concentrated to dryness under vacuum. The residue is crystallized from ethyl acetate/hexane. The title compound melts at 143°-145° C.

후처리

  1. additionis added in small increments
  2. washwashed with 2N hydrochloric acid and water
  3. dry with materialthe dichloromethane solution is dried over sodium sulfate
  4. concentrationconcentrated to dryness under vacuum
  5. customThe residue is crystallized from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-a6fedd8e9f7a413da2a41d0ee8a8f102
출처 데이터셋
uspto-grants-1993_05
특허 번호
US05210290

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