Hydrochloric Acid → 7-Methoxy-isoquinoline-N-oxide hydrochloride

HRID 1279070ノート

反応式

HRID 1279070 の反応式
[Cl:1]C1C=C(C=CC=1)C(OO)=[O:6].[CH3:12][O:13][C:14]1[CH:23]=[C:22]2[C:17]([CH:18]=[CH:19][N:20]=[CH:21]2)=[CH:16][CH:15]=1.CO.Cl>ClCCl.C(OCC)C>[ClH:1].[CH3:12][O:13][C:14]1[CH:23]=[C:22]2[C:17]([CH:18]=[CH:19][N+:20]([O-:6])=[CH:21]2)=[CH:16][CH:15]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 70297m-Chloroperbenzoic acidHCID 5943757-Methoxyisoquinoline

生成物 1

HCID 226656837-Methoxy-isoquinoline-N-oxide hydrochloride

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 6344Dichloromethane溶媒

実験手順

At room temperature 58 g of m-chloroperoxybenzoic acid (purity 75%) were added in portions to a stirred solution of 7-methoxy-isoquinoline (35.9 g) in 500 mL of dichloromethane. Stirring was continued for 3 hours and subsequently methanol (400 mL) was added. The bulk was reduced to 300 mL and 325 mL of a saturated solution of hydrogen chloride in diethyl ether were added. Dilution with 600 mL of diethyl ether afforded precipitation of yellow crystals, which were separated by filtration, washed with chilled diethyl ether and dried in vacuo. Yield: 41.3 g (87%); m.p. 185-187° C.; (+)-FAB-MS: 176 (MH+-HCl).

後処理

  1. additionwere added
  2. customprecipitation of yellow crystals, which
  3. customwere separated by filtration
  4. washwashed with chilled diethyl ether
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-f2505b98de844977a6b03d5c3ae24329
出典データセット
uspto-grants-2002_09
特許番号
US06444672B1

反応ノート

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