1-(2-Nitro-6,7-dihydropyrazolo[1,5-a]pyrazin-5(4H)-yl)ethanone → 1-(2-amino-6,7-dihydropyrazolo[1,5-a]pyrazin-5(4H)-yl)ethanone

HRID 1021685노트

반응식

HRID 1021685 반응식
[N+:1]([C:4]1[CH:15]=[C:7]2[CH2:8][N:9]([C:12](=[O:14])[CH3:13])[CH2:10][CH2:11][N:6]2[N:5]=1)([O-])=O>[Pd].C(O)C>[NH2:1][C:4]1[CH:15]=[C:7]2[CH2:8][N:9]([C:12](=[O:14])[CH3:13])[CH2:10][CH2:11][N:6]2[N:5]=1

참가 물질

4

반응물 1

HCID 580439581-(2-Nitro-6,7-dihydropyrazolo[1,5-a]pyrazin-5(4H)-yl)ethanone

생성물 1

HCID 580440081-(2-amino-6,7-dihydropyrazolo[1,5-a]pyrazin-5(4H)-yl)ethanone수율 95%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

A 500-mL Parr hydrogenation bottle was charged with 125e (2.3 g, 10.9 mmol), 10% palladium on carbon (50% wet, 570 mg dry weight) and ethanol (100 mL). The bottle was evacuated, charged with hydrogen gas to a pressure of 50 psi and shaken for 2 h on a Parr hydrogenation apparatus. The catalyst was removed by filtration through a pad of CELITE® 521 washing with 1:1 CH2Cl2:MeOH (500 mL). The resulting solution was concentrated under reduced pressure to afford a 95% yield (1.9 g) of crude 125f.

후처리

  1. customThe bottle was evacuated
  2. additioncharged with hydrogen gas to a pressure of 50 psi
  3. customThe catalyst was removed by filtration through a pad of CELITE® 521 washing with 1:1 CH2Cl2
  4. concentrationThe resulting solution was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-ca4fea3792b344938369d30f9fb7aad2
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716274B2

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