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Water → Tert-butyl 4-(aminomethyl)-4-benzylsulfanylpiperidine-1-carboxylate

HRID 453582
ノート
印刷プレビュー

反応式

HRID 453582 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([S:14][C:15]1([CH2:28][N+:29]([O-])=O)[CH2:20][CH2:19][N:18]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:17][CH2:16]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O>C(OCC)C.O1CCCC1.C(OCC)(=O)C>[NH2:29][CH2:28][C:15]1([S:14][CH2:7][C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH2:16][CH2:17][N:18]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])[CH2:19][CH2:20]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 962WaterHCID 21226445Aluminium lithium hydride2 回HCID 57475998Tert-butyl 4-(benzylthio)-4-(nitromethyl)piperidine-1-carboxylate

生成物 1

HCID 57475999Tert-butyl 4-(aminomethyl)-4-benzylsulfanylpiperidine-1-carboxylate収率 28.1%

試薬・触媒・溶媒 3

HCID 3283Diethyl Ether溶媒2 回
HCID 8028
Tetrahydrofuran
溶媒
HCID 8857Ethyl Acetate溶媒2 回

実験手順

To a mixture of lithium aluminum hydride (0.4 g) and diethyl ether (20 mL) was added a solution of tert-butyl 4-(benzylthio)-4-(nitromethyl)piperidine-1-carboxylate (1.28 g) in diethyl ether (5 mL) at 0° C. The reaction mixture was heated under reflux for 1 hr. Ethyl acetate was added to decompose excess lithium aluminum hydride, and then water was added. The reaction mixture was diluted with a mixed solvent of tetrahydrofuran and ethyl acetate, and the inorganic salt was removed by filtration. The filtrate was washed with saturated brine, dried (MgSO4) and concentrated. The obtained residue was subjected to silica gel column chromatography to give the title compound (0.33 g, yield 28%) as a colorless oil from a fraction eluted with ethyl acetate-methanol (2:1, volume ratio).

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureunder reflux for 1 hr
  3. customthe inorganic salt was removed by filtration
  4. washThe filtrate was washed with saturated brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-c751a4213cf74a9391817d1ab0f908bf
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08492405B2

反応ノート

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