Water → HCID 58267997, 화합물

HRID 2283669노트

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HRID 2283669 반응식
[H-].[Na+].[Br:3][C:4]1[CH:12]=[C:11]2[C:7]([CH:8]=[N:9][NH:10]2)=[C:6]([N+:13]([O-:15])=[O:14])[CH:5]=1.[CH3:16]I.O>CN(C=O)C>[Br:3][C:4]1[CH:12]=[C:11]2[C:7]([CH:8]=[N:9][N:10]2[CH3:16])=[C:6]([N+:13]([O-:15])=[O:14])[CH:5]=1.[Br:3][C:4]1[CH:5]=[C:6]([N+:13]([O-:15])=[O:14])[C:7]2[C:11]([CH:12]=1)=[N:10][N:9]([CH3:16])[CH:8]=2

참가 물질

7

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 247280596-bromo-4-nitro-1H-indazole

생성물 2

HCID 58267997HCID 58267997, 화합물HCID 903087036-bromo-2-methyl-4-nitro-2H-indazole

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

60% Sodium hydride (including 40% liquid paraffin as an additive) (213 mg) was added to a solution of 6-bromo-4-nitro-1H-indazole (901 mg) in DMF (19 ml) in an ice bath. Subsequently, the reaction solution was stirred at 0° C. for 15 minutes, then methyl iodide (0.35 ml) was added, and the reaction solution was allowed to react at room temperature for 11 hours. The reaction solution was poured into water, and the deposited precipitate was filtrated to obtain a crude product. The crude product was purified by column chromatography on silica gel (developing solvent:hexane/ethyl acetate) to obtain 6-bromo-1-methyl-4-nitro-1H-indazole and 6-bromo-2-methyl-4-nitro-2H-indazole as a yellow solid, respectively.

후처리

  1. customto react at room temperature for 11 hours
  2. filtrationthe deposited precipitate was filtrated
  3. customto obtain a crude product
  4. customThe crude product was purified by column chromatography on silica gel (developing solvent:hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-cbd09c06eb044f8cad96773192b6ea41
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09145414B2

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