Picolinoyl Chloride Hydrochloride → N-(5-Bromo-4-(trifluoromethyl)thiazol-2-yl)picolinamide
反応式
[Br:1][C:2]1[S:6][C:5]([NH2:7])=[N:4][C:3]=1[C:8]([F:11])([F:10])[F:9].Cl.[N:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[C:19](Cl)=[O:20]>C(Cl)Cl>[Br:1][C:2]1[S:6][C:5]([NH:7][C:19](=[O:20])[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][N:13]=2)=[N:4][C:3]=1[C:8]([F:11])([F:10])[F:9]参加物
4
実験手順
To a stirred solution of 5-bromo-4-(trifluoromethyl)thiazol-2-amine (0.204 g, 0.826 mmol) ethyldiisopropylamine (0.36 mL, 2.1 mmol) in methylene chloride (4 mL) at 0° C. was added picolinoyl chloride hydrochloride (0.162 g, 0.908 mmol) and the reaction mixture was stirred at room temperature for 15 h. The reaction mixture was diluted with methylene chloride and washed with saturated NaHCO3, dried, filtered and concentrated under vacuum to give the crude product. The residue was purified by column chromatography eluting with ethyl acetate/hexanes 0 to 30% to give the product.
後処理
- washwashed with saturated NaHCO3
- customdried
- filtrationfiltered
- concentrationconcentrated under vacuum
出典と根拠
- ORDレコード
- ord-c2f87ae475744f28b6b9d3053afc284e
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09192603B2
反応ノート
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