Pyridine → HCID 67520897、化合物

HRID 1925761ノート

反応式

HRID 1925761 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[S:10](Cl)(=[O:12])=[O:11].[NH2:14][C:15]1[CH:19]=[CH:18][S:17][C:16]=1[C:20]([O:22][CH3:23])=[O:21].N1C=CC=CC=1>CN(C)C1C=CN=CC=1.ClCCl>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([F:9])=[CH:4][C:3]=1[S:10]([NH:14][C:15]1[CH:19]=[CH:18][S:17][C:16]=1[C:20]([O:22][CH3:23])=[O:21])(=[O:12])=[O:11]

参加物

6

反応物 3

HCID 1049PyridineHCID 89652Methyl 3-amino-2-thiophenecarboxylateHCID 27735232-Chloro-4,5-difluorobenzenesulfonyl chloride

生成物 1

HCID 67520897HCID 67520897、化合物収率 33.5%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

Synthesized as described for 3 using 2-chloro-4,5,-difluorobenzenesulfonyl chloride (500 mg; 2.02 mmol), methyl 3-aminothiophene-2-carboxylate (382 mg; 2.43 mmol), 4-dimethylaminopyridine (62 mg; 0.51 mmol), pyridine (10 mL), and anhydrous dichloromethane (10 mL). The crude product was purified by automated silica gel chromatography (Biotage®) using ethyl acetate/hexanes as eluant system (0 to 20% v/v over 7 column volume gradient elution) to yield the title product as a white solid (249 mg).

後処理

  1. customSynthesized
  2. customThe crude product was purified by automated silica gel chromatography (Biotage®)
  3. washsystem (0 to 20% v/v over 7 column volume gradient elution)

出典と根拠

ORDレコード
ord-a94fb0826cc84b0b8a12c2112b413dff
出典データセット
uspto-grants-2012_05
特許番号
US08178699B2

反応ノート

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