Hydrazine hydrate (1:1) → HCID 178489372、化合物

HRID 886614ノート

反応式

HRID 886614 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[O:17][CH3:18])=O)[C:5](F)=[N:6][CH:7]=1.O.[NH2:20][NH2:21]>C(O)C>[Br:1][C:2]1[CH:3]=[C:4]2[C:9]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[O:17][CH3:18])=[N:21][NH:20][C:5]2=[N:6][CH:7]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 59825042(5-Bromo-2-fluoro-pyridin-3-yl)-(2-methoxy-phenyl)-methanone

生成物 1

HCID 178489372HCID 178489372、化合物収率 59.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of (5-bromo-2-fluoro-pyridin-3-yl)-(2-methoxy-phenyl)-methanone (1.9 g, 6.1 mmol) in ethanol (125 ml), hydrazine monohydrate (691 μl, 12.2 mmol) was added and the resulting solution was allowed to stir at room temperature overnight. Solvent was removed under reduced pressure and the product was precipitated out by addition of water to afford 5-bromo-3-(2-methoxy-phenyl)-1H-pyrazolo[3,4-b]pyridine (1.1 g, 58% yield). 1H NMR (500 MHz, DMSO-d6) δ 3.84 (s, 3H), 7.07 (m, 1H), 7.20 (d, 1H), 7.45 (m, 1H), 7.62 9d, 1H), 8.34 (s, 1H), 8.60 (s, 1H). MS: m/z 304+306 (M+H+).

後処理

  1. customSolvent was removed under reduced pressure
  2. customthe product was precipitated out by addition of water

出典と根拠

ORDレコード
ord-40d66947a7b4475995b3bf1fb3ee00a0
出典データセット
uspto-grants-2012_08
特許番号
US08242280B2

反応ノート

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