N-bromobutanimide → 5-broMo-3-(trifluoroMethoxy)pyridin-2-aMine
反応式
[F:1][C:2]([F:12])([F:11])[O:3][C:4]1[C:5]([NH2:10])=[N:6][CH:7]=[CH:8][CH:9]=1.[Br:13]N1C(=O)CCC1=O>ClCCl>[Br:13][C:8]1[CH:9]=[C:4]([O:3][C:2]([F:1])([F:11])[F:12])[C:5]([NH2:10])=[N:6][CH:7]=1参加物
4
実験手順
To a solution of 3-(trifluoromethoxy)pyridin-2-amine (300 mg, 1.68 mmol) in dichloromethane (8 mL) was added N-bromosuccinimide (450 mg, 2.53 mmol) at 20° C. The reaction mixture was stirred at the same temperature for another 5 min and subsequently concentrated to dryness in vacuo. The resulting residue was purified by column chromatography (silica gel, 100-200 mesh, 15% ethyl acetate in petroleum ether) affording product (220 mg, 51%): 1H NMR (400 MHz, DMSO-d6) δ 8.03 (d, J=2.0 Hz, 1H), 7.75-7.74 (m, 1H), 6.68 (brs, 2H).
後処理
- concentrationsubsequently concentrated to dryness in vacuo
- customThe resulting residue was purified by column chromatography (silica gel, 100-200 mesh, 15% ethyl acetate in petroleum ether)
出典と根拠
- ORDレコード
- ord-a2785ba5e9cd4888893f89ad5ee35328
- 出典データセット
- uspto-grants-2016_06
- 特許番号
- US09365583B2
反応ノート
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