Pyridine → HCID 53972694、化合物

HRID 248750

反応式

HRID 248750 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 53972694HCID 53972694、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a6fedd8e9f7a413da2a41d0ee8a8f102
出典データセット
uspto-grants-1993_05
特許番号
US05210290

関連ノート

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