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tert-Butyl [1,2,4]triazolo[1,5-a]pyrazin-2-ylcarbamate → tert-Butyl (5,6,7,8-tetrahydro-[1,2,4]triazolo[1,5-a]pyrazin-2-yl)carbamate

HRID 1411973
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인쇄 미리보기

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HRID 1411973 반응식
[C:1]([O:5][C:6](=[O:17])[NH:7][C:8]1[N:16]=[C:11]2[CH:12]=[N:13][CH:14]=[CH:15][N:10]2[N:9]=1)([CH3:4])([CH3:3])[CH3:2]>[Pd].C(O)C>[N:16]1[C:8]([NH:7][C:6](=[O:17])[O:5][C:1]([CH3:3])([CH3:2])[CH3:4])=[N:9][N:10]2[CH2:15][CH2:14][NH:13][CH2:12][C:11]=12
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 89548973tert-Butyl [1,2,4]triazolo[1,5-a]pyrazin-2-ylcarbamate

생성물 1

HCID 86684511tert-Butyl (5,6,7,8-tetrahydro-[1,2,4]triazolo[1,5-a]pyrazin-2-yl)carbamate수율 68.8%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

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온도
60 °C

실험 절차

A 100-mL round-bottomed flask was purged with nitrogen and charged with 270c (1.0 g, 4.25 mmol), 20% palladium on carbon (10% wet, 200 mg), and ethanol (40 mL). It was then evacuated, charged with hydrogen gas (25 atm), and stirred at 60° C. for 24 h. The hydrogen was evacuated and nitrogen was charged into the flask. The catalyst was removed by filtration through a pad of CELITE® and the filtrate was concentrated under reduced pressure to afford 270d (700 mg, 68%). MS-ESI: [M-t-Bu]+ 184.0

후처리

  1. customA 100-mL round-bottomed flask was purged with nitrogen
  2. customIt was then evacuated
  3. additioncharged with hydrogen gas (25 atm)
  4. customThe hydrogen was evacuated
  5. additionnitrogen was charged into the flask
  6. customThe catalyst was removed by filtration through a pad of CELITE®
  7. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-d9fb9308718a4d12a99ce1957688b88c
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08921353B2

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