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Ethanol → tert-butyl 4-(3-phenyl-1H-pyrazol-5-yl)piperidine-1-carboxylate

HRID 222250
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HRID 222250 반응식
O=[C:2]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:3][C:4]([CH:6]1[CH2:11][CH2:10][N:9]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:8][CH2:7]1)=O.O.[NH2:26][NH2:27].C(O)C>C1COCC1>[C:19]1([C:2]2[CH:3]=[C:4]([CH:6]3[CH2:11][CH2:10][N:9]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:8][CH2:7]3)[NH:27][N:26]=2)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 24654Hydrazine hydrate (1:1)3회HCID 49760127tert-Butyl 4-(3-oxo-3-phenylpropanoyl)piperidine-1-carboxylate

생성물 1

HCID 67109296tert-butyl 4-(3-phenyl-1H-pyrazol-5-yl)piperidine-1-carboxylate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of tert-butyl 4-(3-oxo-3-phenylpropanoyl)piperidine-1-carboxylate (3.1 g), hydrazine monohydrate (0.5 mL), ethanol (30 mL), and THF (30 mL) was stirred at room temperature for about 15 hours, and at 60° C. for 1 hour. Hydrazine monohydrate (0.5 mL) was further added thereto, followed by stirring again at 60° C. for 3 hours. Hydrazine monohydrate (4.0 mL) was added thereto again, followed by stirring at 60° C. for 8 hours. After leaving to be cooled, the solvent was evaporated under reduced pressure, and to the residue were added diisopropyl ether and methanol, followed by stirring. The resulting solid was collected by filtration and dried under reduced pressure to obtain tert-butyl 4-(3-phenyl-1H-pyrazol-5-yl)piperidine-1-carboxylate (2.46 g).

후처리

  1. waitat 60° C. for 1 hour
  2. stirringby stirring again at 60° C. for 3 hours
  3. stirringby stirring at 60° C. for 8 hours
  4. customAfter leaving
  5. temperatureto be cooled
  6. customthe solvent was evaporated under reduced pressure
  7. additionto the residue were added diisopropyl ether and methanol
  8. stirringby stirring
  9. filtrationThe resulting solid was collected by filtration
  10. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-4edd8abd079f425ab29f50450bbf513d
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08207199B2

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