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Piperidine → HCID 12471526、化合物

HRID 2051481
ノート
印刷プレビュー

反応式

HRID 2051481 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 12471526HCID 12471526、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-3b5c1d99455d418b9379f07dabe99adc
出典データセット
uspto-grants-1991_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05019574

反応ノート

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