(4aRS,5SR,8aRS)-1-Benzyl-5-(benzylamino)perhydroquinoxaline-2,3-dione → (4aRS,5SR,8aRS)-5-amino-1-benzylperhydroquinoxaline-2,3-dione

HRID 1876799

반응식

HRID 1876799 반응식
[CH2:1]([N:8]1[CH:17]2[CH:12]([CH:13]([NH:18]CC3C=CC=CC=3)[CH2:14][CH2:15][CH2:16]2)[NH:11][C:10](=[O:26])[C:9]1=[O:27])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>CO.[Pd]>[NH2:18][CH:13]1[CH2:14][CH2:15][CH2:16][CH:17]2[CH:12]1[NH:11][C:10](=[O:26])[C:9](=[O:27])[N:8]2[CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 1

HCID 68775989(4aRS,5SR,8aRS)-1-Benzyl-5-(benzylamino)perhydroquinoxaline-2,3-dione

생성물 1

HCID 68777664(4aRS,5SR,8aRS)-5-amino-1-benzylperhydroquinoxaline-2,3-dione

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

(4aRS,5SR,8aRS)-1-Benzyl-5-(benzylamino)perhydroquinoxaline-2,3-dione (1.19 g, 3.28 mmol) was dissolved in methanol (40 ml) and NH4HCO2 (2.07 g, 32.8 mmol) was added. 120 mg of palladium-on-carbon (Merck) was furthermore added. The mixture was heated under reflux for 2 hours. The catalyst was then filtered off and the mixture was evaporated in vacuo. The residue was taken up in CH2Cl2 and the mixture was washed three times with 0.1 N NaOH. The organic phase was dried over Na2SO4 and evaporated in vacuo. A colorless solid was obtained.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 2 hours
  3. filtrationThe catalyst was then filtered off
  4. customthe mixture was evaporated in vacuo
  5. washthe mixture was washed three times with 0.1 N NaOH
  6. dry with materialThe organic phase was dried over Na2SO4
  7. customevaporated in vacuo
  8. customA colorless solid was obtained

출처 및 근거

ORD 기록
ord-d09017786fd64c849cb81b4d421530a0
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08309725B2

연결된 노트

불러오는 중…