2,3-Dichloropyrazine → 4-(3-Chloro-pyrazin-2-ylamino)-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide

HRID 20290

反応式

HRID 20290 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]([C:11]2[C:15]([NH2:16])=[CH:14][NH:13][N:12]=2)=[O:10])=[CH:4][CH:3]=1.[Cl:17][C:18]1[C:23](Cl)=[N:22][CH:21]=[CH:20][N:19]=1>>[F:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9]([C:11]2[C:15]([NH:16][C:23]3[C:18]([Cl:17])=[N:19][CH:20]=[CH:21][N:22]=3)=[CH:14][NH:13][N:12]=2)=[O:10])=[CH:6][CH:7]=1

参加物

3

反応物 2

HCID 785752,3-DichloropyrazineHCID 178508056HCID 178508056、化合物

生成物 1

HCID 1785221454-(3-Chloro-pyrazin-2-ylamino)-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide収率 19.6%

実験手順

A mixture of 4-amino-1H-pyrazole-3-carboxylic acid (4-fluoro-phenyl)-amide (50 mg; 0.23 mmol) and 2,3-dichloropyrazine (140 mg; 0.92 mmol) was heated at 150° C. (50W) for 20 minutes in a CEM Discover™ microwave synthesiser. The crude reaction mixture was purified by flash column chromatography eluting with ethyl acetate/hexane (1:3 then 1:2). Product containing fractions were combined and evaporated to give 15 mg of the title compound as a white solid. (LC/MS: Rt 4.06 M+H]+ 332).

後処理

  1. customThe crude reaction mixture
  2. customwas purified by flash column chromatography
  3. washeluting with ethyl acetate/hexane (1:3
  4. additionProduct containing fractions
  5. customevaporated

出典と根拠

ORDレコード
ord-8c5cbc49edc048d6a9099255935e52f9
出典データセット
uspto-grants-2010_06
特許番号
US07745638B2

関連ノート

読み込み中…