Methanol → 5-bromo-6-methoxyisoquinoline-N-oxide hydrochloride

HRID 1436011

反応式

HRID 1436011 の反応式
[Cl:1]C1C=CC=C(C(OO)=[O:9])C=1.[Br:12][C:13]1[C:22]([O:23][CH3:24])=[CH:21][CH:20]=[C:19]2[C:14]=1[CH:15]=[CH:16][N:17]=[CH:18]2.CO>ClCCl>[ClH:1].[Br:12][C:13]1[C:22]([O:23][CH3:24])=[CH:21][CH:20]=[C:19]2[C:14]=1[CH:15]=[CH:16][N+:17]([O-:9])=[CH:18]2

参加物

5

反応物 3

HCID 887MethanolHCID 70297m-Chloroperbenzoic acidHCID 222265455-Bromo-6-methoxy-isoquinoline

生成物 1

HCID 688780245-bromo-6-methoxyisoquinoline-N-oxide hydrochloride収率 83.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

m-Chloroperbenzoic acid (1.4 g, 75%) was added in portions to a stirred solution of 5-bromo-6-methoxyisoquinoline (12 g, 5.04 mmol) in dichloromethane (12 ml). The mixture was stirred for 1 h then further dichloromethane (10 ml) added and the mixture stirred for an additional 2 h. Methanol (12 ml) was added and the mixture concentrated in vacuo to ˜9 ml, then 1M hydrochloric acid in diethyl ether (10 ml) was added. The mixture was diluted with ether and filtered, the precipitated solid was washed with diethyl ether and dried in vacuo to give crude 5-bromo-6-methoxyisoquinoline-N-oxide hydrochloride (1.22 g).

後処理

  1. stirringthe mixture stirred for an additional 2 h
  2. concentrationthe mixture concentrated in vacuo to ˜9 ml
  3. addition1M hydrochloric acid in diethyl ether (10 ml) was added
  4. additionThe mixture was diluted with ether
  5. filtrationfiltered
  6. washthe precipitated solid was washed with diethyl ether
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-a3cddaab01a94e84accae8268c62de9f
出典データセット
uspto-grants-2009_11
特許番号
US07618985B2

関連ノート

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