Potassium Carbonate → HCID 67976141、化合物

HRID 706653ノート

反応式

HRID 706653 の反応式
[Br:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][C:9]=2[N+:11]([O-:13])=[O:12])[NH:4][N:3]=1.C(=O)([O-])[O-].[K+].[K+].Cl.Cl[CH2:22][C:23]1[CH:28]=[CH:27][CH:26]=[C:25]([O:29][CH2:30][CH3:31])[N:24]=1>CN(C=O)C>[Br:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][C:9]=2[N+:11]([O-:13])=[O:12])[N:4]([CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[C:25]([O:29][CH2:30][CH3:31])[N:24]=2)[N:3]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 67975026HCID 67975026、化合物HCID 178526560HCID 178526560、化合物

生成物 1

HCID 67976141HCID 67976141、化合物収率 52%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 3-bromo-4-nitro-1H-indazole (1.5 g, 6.20 mmol) in DMF (0.5M, 12 mL) was added potassium carbonate (1.71 g, 12.4 mmol) at ambient temperature. After 15 minutes, 2-(chloromethyl)-6-ethoxypyridine hydrochloride (1.29 g, 6.20 mmol) was added. The mixture was allowed to stir at ambient temperature for 18 hours. The mixture was concentrated and diluted with ice-water (300 mL). Precipitated solids were collected by filtration, washed with water and dried under high vacuum overnight to provide 3-bromo-1-((6-ethoxypyridin-2-yl)methyl)-4-nitro-1H-indazole (1.21 g, 52% yield).

後処理

  1. concentrationThe mixture was concentrated
  2. additiondiluted with ice-water (300 mL)
  3. customPrecipitated solids
  4. filtrationwere collected by filtration
  5. washwashed with water
  6. customdried under high vacuum overnight

出典と根拠

ORDレコード
ord-664164314b194bea8391d9c234f0ffd5
出典データセット
uspto-grants-2015_11
特許番号
US09174981B2

反応ノート

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