4-(1-Pyrrolidinyl)piperidine → 2-Phenyl-3-pyrid-4-yl-6-(4-pyrrolidin-1-ylpiperid-1-yl)imidazo[1,2-b]pyridazine

HRID 1803903

반응식

HRID 1803903 반응식
Cl[C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8]([C:17]3[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=3)=[C:9]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=3)[N:10]=2)[N:7]=1.[N:23]1([CH:28]2[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]2)[CH2:27][CH2:26][CH2:25][CH2:24]1>C(O)C>[C:11]1([C:9]2[N:10]=[C:5]3[CH:4]=[CH:3][C:2]([N:31]4[CH2:32][CH2:33][CH:28]([N:23]5[CH2:27][CH2:26][CH2:25][CH2:24]5)[CH2:29][CH2:30]4)=[N:7][N:6]3[C:8]=2[C:17]2[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

참가 물질

4

반응물 2

HCID 787034-(1-Pyrrolidinyl)piperidineHCID 594069546-Chloro-2-phenyl-3-pyrid-4-ylimidazo[1,2-b]pyridazine

생성물 1

HCID 594069552-Phenyl-3-pyrid-4-yl-6-(4-pyrrolidin-1-ylpiperid-1-yl)imidazo[1,2-b]pyridazine수율 27%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
155 °C

실험 절차

A mixture of 4.03 g (13.1 mmol) of 6-chloro-2-phenyl-3-pyrid-4-ylimidazo[1,2-b]pyridazine and 4.4 g (29 mmol) of 4-pyrrolidin-1-ylpiperidine in 50 mL of ethanol is heated at 155° C. for 4 hours. After cooling, the solvent is evaporated off under reduced pressure and the residue is chromatographed on silica gel, eluting with a mixture of dichloromethane and methanol (93:7). The product is then recrystallized from 40 mL of methanol to give 1.5 g of yellow crystals after drying under reduced pressure.

후처리

  1. temperatureAfter cooling
  2. customthe solvent is evaporated off under reduced pressure
  3. customthe residue is chromatographed on silica gel
  4. washeluting with a mixture of dichloromethane and methanol (93:7)
  5. customThe product is then recrystallized from 40 mL of methanol

출처 및 근거

ORD 기록
ord-d74563b07826453e8a6b0f5a747daba8
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08354405B2

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