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Tert-butyl(4-benzylpiperazin-1-yl)carbamate → tert-Butyl piperazin-1-ylcarbamate

HRID 856033
ノート
印刷プレビュー

反応式

HRID 856033 の反応式
[C:1]([O:5][C:6](=[O:21])[NH:7][N:8]1[CH2:13][CH2:12][N:11](CC2C=CC=CC=2)[CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2].[H][H]>C(O)C.[OH-].[OH-].[Pd+2]>[N:8]1([NH:7][C:6](=[O:21])[O:5][C:1]([CH3:3])([CH3:2])[CH3:4])[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 23081385Tert-butyl(4-benzylpiperazin-1-yl)carbamateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 21701658tert-Butyl piperazin-1-ylcarbamate収率 99%

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 702Ethanol溶媒

実験手順

Tert-butyl(4-benzylpiperazin-1-yl)carbamate (42.22 g, 145 mmol) prepared in Reference Example 35 was dissolved in ethanol (300 ml). To which 20% palladium hydroxide/carbon (6.0 g) was added, and the mixture was stirred at room temperature under an atmospheric pressure of hydrogen for 20 minutes, and then at 50° C. for 30 minutes. The catalyst was removed by filtration, and the filtrate was concentrated under reduced pressure. Thus obtained solid was washed with IPE, collected by filtration, and dried under reduced pressure to afford tert-butyl piperazin-1-yl-carbamate (28.9 g, yield 99%) as a colorless crystalline powder.

後処理

  1. customThe catalyst was removed by filtration
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. washThus obtained solid was washed with IPE
  4. filtrationcollected by filtration
  5. customdried under reduced pressure

出典と根拠

ORDレコード
ord-88382c786981466c9830c93761e911bd
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07262212B2

反応ノート

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