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

HRID 357331노트

반응식

HRID 357331 반응식
[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

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 14823453HCID 14823453, 화합물

생성물 1

HCID 148234453-(Piperazin-1-YL)-1H-indazole수율 73%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b7a8770517484b7fa3d0d9648b774a11
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840727

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