Water → HCID 14823453、化合物

HRID 1955841ノート

反応式

HRID 1955841 の反応式
[N:1]#[C:2]Br.C[N:5]1[CH2:10][CH2:9][N:8]([C:11]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[NH:13][N:12]=2)[CH2:7][CH2:6]1.O>CS(C)=O>[NH:13]1[C:14]2[C:19](=[CH:18][CH:17]=[CH:16][CH:15]=2)[C:11]([N:8]2[CH2:7][CH2:6][N:5]([C:2]#[N:1])[CH2:10][CH2:9]2)=[N:12]1

参加物

5

反応物 3

HCID 962WaterHCID 10476Cyanogen BromideHCID 148234523-(4-Methylpiperazin-1-yl)-1H-indazole

生成物 1

HCID 14823453HCID 14823453、化合物

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒2 回

実験手順

To a stirred mixture of cyanogen bromide (5.3 g, 0.05 mol), K2 CO3 (7.1 g) and dimethylsulfoxide (40 ml) was added, dropwise, 3-(4-methyl-1-piperazinyl)-1H-indazole (1 1.0 g 0.051 mol) dissolved in dimethylsulfoxide (60 ml). The reaction was stirred at ambient temperature for 1 hour, and then it was poured into water. The aqueous suspension was extracted with ethyl acetate, the ethyl acetate was washed (H2O), dried (MgSO4), and concentrated to afford 7.8 g (67%) of a ye llow solid. This sample was combined with another and recrystallized twice from toluene to afford analytically pure 4-(1H-indazol-3-yl)-1-piperazinecarbonitrile as a white solid, m.p.=12°-122° C.

後処理

  1. additionwas added
  2. extractionThe aqueous suspension was extracted with ethyl acetate
  3. washthe ethyl acetate was washed (H2O)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated
  6. customto afford 7.8 g (67%) of a ye llow solid
  7. customrecrystallized twice from toluene

出典と根拠

ORDレコード
ord-4aff8aba31e2430a9cf103fa14246ed7
出典データセット
uspto-grants-1998_07
特許番号
US05776963

反応ノート

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