Picolinoyl Chloride Hydrochloride → N-(5-Bromo-4-(trifluoromethyl)thiazol-2-yl)picolinamide

HRID 716621ノート

反応式

HRID 716621 の反応式
[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

  1. washwashed with saturated NaHCO3
  2. customdried
  3. filtrationfiltered
  4. 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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