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

HRID 251584노트

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HRID 251584 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 174Ethylene Glycol용매

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온도
160 °C

실험 절차

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 hours 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).

후처리

  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

출처 및 근거

ORD 기록
ord-13b1ee70a3544861a3f03397d0316c7d
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07863454B2

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