Water → 4-Bromo-3-isopropyl-1H-indazole

HRID 1091923ノート

反応式

HRID 1091923 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4](F)[C:3]=1[C:9](=O)[CH:10]([CH3:12])[CH3:11].[NH2:14][NH2:15].O>C(O)CO>[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]2[C:3]=1[C:9]([CH:10]([CH3:12])[CH3:11])=[N:14][NH:15]2

参加物

5

反応物 3

HCID 962WaterHCID 9321HydrazineHCID 665895481-(2-Bromo-6-fluorophenyl)-2-methylpropan-1-one

生成物 1

HCID 1784404044-Bromo-3-isopropyl-1H-indazole

試薬・触媒・溶媒 1

HCID 174Ethylene Glycol溶媒

反応条件

温度
160 °C

実験手順

A mixture of 1-(2-bromo-6-fluoro-phenyl)-2-methyl-propan-1-one (1.1 g, 4.5 mmol) and anhydrous hydrazine (0.17 mL, 5.4 mmol) in ethylene glycol (10 mL) is heated for 16 h at 160° C. Water is added and the mixture is extracted with CH2Cl2. The combined extracts are dried (MgSO4) and concentrated in vacuo. The residue is purified by flash chromatography to yield 4-bromo-3-isopropyl-1H-indazole. 1H NMR (CDCl3) 10.1 (br s, 1H), 7.38 (d, 1H), 7.32 (d, 1H), 7.17 (t, 1H), 3.99 (m, 1H), 1.43 (d, 6H).

後処理

  1. extractionthe mixture is extracted with CH2Cl2
  2. dry with materialThe combined extracts are dried (MgSO4)
  3. concentrationconcentrated in vacuo
  4. customThe residue is purified by flash chromatography

出典と根拠

ORDレコード
ord-bffe12baf6aa4176a42d9ae1327c714c
出典データセット
uspto-grants-2012_03
特許番号
US08129395B2

反応ノート

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