HCID 22614896, 화합물 → 5-Amino-6,7-dichloro-2,3-dimethoxyquinoxaline

HRID 842702노트

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HRID 842702 반응식
[Cl:1][C:2]1[C:3]([N+:17]([O-])=O)=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[N:8]=[C:7]([O:13][CH3:14])[C:6]([O:15][CH3:16])=[N:5]2>O1CCCC1.C(OCC)(=O)C.ClCCl.[Pd]>[NH2:17][C:3]1[C:2]([Cl:1])=[C:11]([Cl:12])[CH:10]=[C:9]2[C:4]=1[N:5]=[C:6]([O:15][CH3:16])[C:7]([O:13][CH3:14])=[N:8]2

참가 물질

6

반응물 1

HCID 22614896HCID 22614896, 화합물

생성물 1

HCID 106066205-Amino-6,7-dichloro-2,3-dimethoxyquinoxaline수율 78.5%

시약·촉매·용매 4

HCID 23938Palladium촉매HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

6,7-Dichloro-2,3-dimethoxy-5-nitroquinoxaline (20 g, 0.066 mol) and 5% w/w palladium-on-carbon (50% wet) (1.2 g) were suspended in a mixture of tetrahydrofuran (0.12 L) and ethyl acetate (0.12 L). The mixture was hydrogenated at 60° C. and 414 kPa (60 psi) for 22 hours, cooled, diluted with dichloromethane (0.48 L) and the catalyst removed by filtration through celite (trade mark) filter aid. The solution was concentrated under reduced pressure with the gradual addition of toluene. The mixture was then filtered and the solid was washed with toluene (20 ml) to give the title compound as a brown solid (14.2 g, 78%), m.p. 182-4° C.

후처리

  1. customwas hydrogenated at 60° C.
  2. temperaturecooled
  3. customthe catalyst removed by filtration through celite (trade mark)
  4. filtrationfilter aid
  5. concentrationThe solution was concentrated under reduced pressure with the gradual addition of toluene
  6. filtrationThe mixture was then filtered
  7. washthe solid was washed with toluene (20 ml)

출처 및 근거

ORD 기록
ord-61df4a5765e142f98012c1f9ac80c9ee
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06376490B1

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