HCID 22614896、化合物 → 5-Amino-6,7-dichloro-2,3-dimethoxyquinoxaline

HRID 842702ノート

反応式

HRID 842702 の反応式
[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

参加物

6

反応物 1

HCID 22614896HCID 22614896、化合物

生成物 1

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

試薬・触媒・溶媒 4

HCID 23938Palladium触媒HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-61df4a5765e142f98012c1f9ac80c9ee
出典データセット
uspto-grants-2002_04
特許番号
US06376490B1

反応ノート

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