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Benzyl (S)-4-((1-(tert-butoxycarbonyl)piperidin-3-yl)methyl)piperazine-1-carboxylate → tert-butyl (3S)-3-(piperazin-1-ylmethyl)piperidine-1-carboxylate

HRID 2371171
ノート
印刷プレビュー

反応式

HRID 2371171 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH2:11][C@@H:10]([CH2:14][N:15]2[CH2:20][CH2:19][N:18](C(OCC3C=CC=CC=3)=O)[CH2:17][CH2:16]2)[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>CO>[N:15]1([CH2:14][C@@H:10]2[CH2:11][CH2:12][CH2:13][N:8]([C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7])[CH2:9]2)[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 59846076Benzyl (S)-4-((1-(tert-butoxycarbonyl)piperidin-3-yl)methyl)piperazine-1-carboxylate

生成物 1

HCID 24886660tert-butyl (3S)-3-(piperazin-1-ylmethyl)piperidine-1-carboxylate収率 99.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Benzyl 4-{[(3S)-1-(tert-butoxycarbonyl)piperidin-3-yl]methyl}piperazine-1-carboxylate (5.0 g, 12.4 mmol) was dissolved in methanol (50 ml) in a three-necked flask. The air was removed under reduced pressure and replaced with argon before the addition of 10% Pd/C (1.24 g). A balloon of hydrogen was then added and the reaction stirred at room temperature for 18 h. The hydrogen was evacuated and replaced with argon. The catalyst was then filtered and the solvent removed under reduced pressure to afford the desired product as a white foam (3.5 g). The compound was used without further purification.

後処理

  1. customThe air was removed under reduced pressure
  2. additionreplaced with argon before the addition of 10% Pd/C (1.24 g)
  3. additionA balloon of hydrogen was then added
  4. customThe hydrogen was evacuated
  5. filtrationThe catalyst was then filtered
  6. customthe solvent removed under reduced pressure

出典と根拠

ORDレコード
ord-0d8b8af7ab294dd59c4c4abb29ec5f39
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08710224B2

反応ノート

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