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Piperidine → HCID 12471526, 화합물

HRID 2051481
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HRID 2051481 반응식
Br[C:2]1[CH:3]=[N+:4]([O-:15])[C:5]2[C:10]([C:11]=1[N+:12]([O-:14])=[O:13])=[CH:9][CH:8]=[CH:7][CH:6]=2.[NH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1>O1CCCC1>[N+:12]([C:11]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N+:4]([O-:15])=[CH:3][C:2]=1[N:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1)([O-:14])=[O:13]
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참가 물질

4

반응물 2

HCID 8082PiperidineHCID 84235Quinoline, 3-bromo-4-nitro-, 1-oxide

생성물 1

HCID 12471526HCID 12471526, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

3-Bromo-4-nitroquinoline-N-oxide (10 g, 0.037 mol) was dissolved in tetrahydrofuran (100 ml). To the solution, piperidine (7.9 g, 0.093 mol) was added and the mixture was stirred at room temperature until gradual crystallization occurred. Tetrahydrofuran was distilled off from the whole reaction mixture under vacuum and the residue was dissolved in chloroform. The chloroform layer was washed with water and dried with anhydrous sodium sulfate. After distilling off the chloroform under vacuum, the residue was washed with a small amount of ethanol and recovered by filtration under vacuum to obtain 4-nitro-3-piperidinoquinoline-N-oxide in an amount of 6.0 g (yield, 59%).

후처리

  1. distillationTetrahydrofuran was distilled off from the whole reaction mixture under vacuum
  2. dissolutionthe residue was dissolved in chloroform
  3. washThe chloroform layer was washed with water
  4. dry with materialdried with anhydrous sodium sulfate
  5. distillationAfter distilling off the chloroform under vacuum
  6. washthe residue was washed with a small amount of ethanol
  7. filtrationrecovered by filtration under vacuum

출처 및 근거

ORD 기록
ord-3b5c1d99455d418b9379f07dabe99adc
출처 데이터셋
uspto-grants-1991_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05019574

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