1-(3,3-Dimethoxypropyl)-7-methoxy-3,4-dihydroquinoxalin-2(1H)one → 1-(3,3-Dimethoxypropyl)-7-methoxyquinoxalin-2(1H)-one

HRID 1847082ノート

反応式

HRID 1847082 の反応式
[CH3:1][O:2][CH:3]([O:19][CH3:20])[CH2:4][CH2:5][N:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([O:16][CH3:17])[CH:14]=2)[NH:9][CH2:8][C:7]1=[O:18]>ClCCl.[O-2].[O-2].[Mn+4]>[CH3:20][O:19][CH:3]([O:2][CH3:1])[CH2:4][CH2:5][N:6]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([O:16][CH3:17])[CH:14]=2)[N:9]=[CH:8][C:7]1=[O:18]

参加物

4

反応物 1

HCID 867250051-(3,3-Dimethoxypropyl)-7-methoxy-3,4-dihydroquinoxalin-2(1H)one

生成物 1

HCID 867249271-(3,3-Dimethoxypropyl)-7-methoxyquinoxalin-2(1H)-one収率 72%

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 6344Dichloromethane溶媒

実験手順

In dichloromethane (10 ml) was dissolved 1-(3,3-dimethoxypropyl)-7-methoxy-3,4-dihydroquinoxalin-2(1H)one (201 mg, 0.717 mmol) under a nitrogen gas atmosphere, manganese dioxide (733 mg, 7.17 mmol) was added thereto at room temperature and the mixture was stirred at the same temperature for 17 hours. The insoluble material was removed by filtration using celite, the filtrate was concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (n-hexane/ethyl acetate) to yield 143 mg (72%) of the title compound in the form of a yellowish solid.

後処理

  1. customThe insoluble material was removed by filtration
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customthe residue was purified by silica gel column chromatography (n-hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-56529800bdd74b0d99adaf9d91dd2be2
出典データセット
uspto-grants-2015_02
特許番号
US08952010B2

反応ノート

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