Sodium Hydroxide → 3-(Piperazin-1-YL)-1H-indazole

HRID 235363ノート

反応式

HRID 235363 の反応式
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([N:10]2[CH2:15][CH2:14][N:13](C#N)[CH2:12][CH2:11]2)=[N:2]1.[OH-].[Na+]>OS(O)(=O)=O>[N:10]1([C:3]2[C:4]3[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=3)[NH:1][N:2]=2)[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 14823453HCID 14823453、化合物

生成物 1

HCID 148234453-(Piperazin-1-YL)-1H-indazole収率 73%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

A mixture of 4-(1H-indazol-3-yl)-1-piperazinecarbonitrile (8.0 g, 40 mmol) and 25% H2SO4 (100 ml) was stirred at reflux for 4.5 hours. The reaction was cooled in an ice bath and made basic by the dropwise addition of 50% NaOH. The basic solution was extracted with ethyl acetate. The ethyl acetate was washed with H2O, dried with MgSO4, and concentrated to afford 5.2 g (73% of the desired compound, as a solid. The solid was recrystallized twice from toluene to afford 3.0 g of 3-(1-piperazinyl)-1H-indazole, m.p.=153°-155° C.

後処理

  1. temperatureat reflux for 4.5 hours
  2. temperatureThe reaction was cooled in an ice bath
  3. extractionThe basic solution was extracted with ethyl acetate
  4. washThe ethyl acetate was washed with H2O
  5. dry with materialdried with MgSO4
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-9dcf1ff86dbc4519b5466a15faa57bb5
出典データセット
uspto-grants-1997_01
特許番号
US05597842

反応ノート

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