Hydrazine hydrate (1:1) → 4-(4-Cyclobutylpiperazin-1-yl)-6-hydrazinopyrimidine

HRID 562452노트

반응식

HRID 562452 반응식
O.[NH2:2][NH2:3].Cl[C:5]1[CH:10]=[C:9]([N:11]2[CH2:16][CH2:15][N:14]([CH:17]3[CH2:20][CH2:19][CH2:18]3)[CH2:13][CH2:12]2)[N:8]=[CH:7][N:6]=1>C(O)C>[CH:17]1([N:14]2[CH2:15][CH2:16][N:11]([C:9]3[CH:10]=[C:5]([NH:2][NH2:3])[N:6]=[CH:7][N:8]=3)[CH2:12][CH2:13]2)[CH2:20][CH2:19][CH2:18]1

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 579250694-Chloro-6-(4-cyclobutylpiperazin-1-yl)pyrimidine

생성물 1

HCID 462211044-(4-Cyclobutylpiperazin-1-yl)-6-hydrazinopyrimidine

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
80 °C

실험 절차

At RT, 4.4 ml (4.5 g, 89.7 mmol) of hydrazine hydrate are added dropwise with stirring to a solution of 1.9 g (7.5 mmol) of 4-chloro-6-(4-cyclobutylpiperazin-1-yl)pyrimidine in 28 ml of ethanol. The reaction solution is stirred at 80° C. for 16 h. For work-up, the mixture is concentrated under reduced pressure, the residue is triturated repeatedly with diethyl ether, and the precipitated solid is filtered off and dried under reduced pressure. The residue is then purified by column chromatography on silica gel (mobile phase dichloromethane/methanol 10/2). Yield: 1.5 g (80% of theory)

후처리

  1. concentrationFor work-up, the mixture is concentrated under reduced pressure
  2. customthe residue is triturated repeatedly with diethyl ether
  3. filtrationthe precipitated solid is filtered off
  4. customdried under reduced pressure
  5. customThe residue is then purified by column chromatography on silica gel (mobile phase dichloromethane/methanol 10/2)

출처 및 근거

ORD 기록
ord-e983cb9e25bb487e93f3de2224459ecd
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08067407B2

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