4-(1-Tert-butoxycarbonyl-piperidin-4-ylmethyl)-3-oxo-piperazine-1-carboxylic acid benzyl ester → 4-(2-Oxo-piperazin-1-ylmethyl)-piperidine-1-carboxylic acid tert-butyl ester

HRID 1433086ノート

反応式

HRID 1433086 の反応式
C(OC([N:11]1[CH2:16][CH2:15][N:14]([CH2:17][CH:18]2[CH2:23][CH2:22][N:21]([C:24]([O:26][C:27]([CH3:30])([CH3:29])[CH3:28])=[O:25])[CH2:20][CH2:19]2)[C:13](=[O:31])[CH2:12]1)=O)C1C=CC=CC=1>CO.[Pd]>[C:27]([O:26][C:24]([N:21]1[CH2:22][CH2:23][CH:18]([CH2:17][N:14]2[CH2:15][CH2:16][NH:11][CH2:12][C:13]2=[O:31])[CH2:19][CH2:20]1)=[O:25])([CH3:30])([CH3:28])[CH3:29]

参加物

4

反応物 1

HCID 234473564-(1-Tert-butoxycarbonyl-piperidin-4-ylmethyl)-3-oxo-piperazine-1-carboxylic acid benzyl ester

生成物 1

HCID 234475144-(2-Oxo-piperazin-1-ylmethyl)-piperidine-1-carboxylic acid tert-butyl ester

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A solution of 4-(1-tert-butoxycarbonyl-piperidin-4-ylmethyl)-3-oxo-piperazine-1-carboxylic acid benzyl ester (2.3 g, 5.4 mmol) in methanol (75 mL) is purged with nitrogen and 10% Pd on carbon (0.3 g) is added, and the reaction is again purged with nitrogen. The reaction is placed on a Parr shaker under hydrogen for 16 h. After the system is purged of hydrogen, the catalyst is filtered and washed with methanol. The filtrate is concentrated to provide 4-(2-oxo-piperazin-1-ylmethyl)-piperidine-1-carboxylic acid tert-butyl ester which is used without further purification. MS (EI) 298 (M+H)+.

後処理

  1. additionis added
  2. customthe reaction is again purged with nitrogen
  3. customAfter the system is purged of hydrogen
  4. filtrationthe catalyst is filtered
  5. washwashed with methanol
  6. concentrationThe filtrate is concentrated

出典と根拠

ORDレコード
ord-da9b6cced0694fb6878e72b9f3d67083
出典データセット
uspto-grants-2009_11
特許番号
US07612075B2

反応ノート

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