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

HRID 856033
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HRID 856033 반응식
[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
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참가 물질

5

반응물 2

HCID 23081385Tert-butyl(4-benzylpiperazin-1-yl)carbamateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 21701658tert-Butyl piperazin-1-ylcarbamate수율 99%

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-88382c786981466c9830c93761e911bd
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07262212B2

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