Hydrochloric Acid → HCID 22397332、化合物

HRID 1070555

反応式

HRID 1070555 の反応式
[Cl:1]C1C=CC=C(C(OO)=[O:9])C=1.[CH3:12][O:13][C:14]1[CH:15]=[C:16]2[C:21](=[CH:22][CH:23]=1)[CH:20]=[N:19][CH:18]=[CH:17]2.CO.Cl>ClCCl.C(OCC)C>[ClH:1].[CH3:12][O:13][C:14]1[CH:15]=[C:16]2[C:21](=[CH:22][CH:23]=1)[CH:20]=[N+:19]([O-:9])[CH:18]=[CH:17]2

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 70297m-Chloroperbenzoic acidHCID 110409786-Methoxyisoquinoline

生成物 1

HCID 22397332HCID 22397332、化合物

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 133 g of m-chloroperbenzoic acid (purity 75%) was added in portions to a stirred solution of 6-methoxy-isoquinoline [Hendrickson, J. B.; Rodriguez, C.; J. Org. Chem. 1983, 48, 3344-3346; 79.8 g; 500 mmol] in 1.2 L of dichloromethane. Stirring was continued for 3 hours and subsequently methanol (1 L) was added. The bulk was reduced to 700 mL after which 800 mL of a saturated solution of hydrogen chloride in diethyl ether was added. Dilution with 1.5 L of diethyl ether resulted in precipitation of yellow crystals, which were separated by filtration, washed with chilled diethyl ether and dried in vacuo. Yield: 85 g (80%); white solid; m.p. 189-191° C.; (+)-FAB-MS: 176 (MH+-HCl).

後処理

  1. additionwas added
  2. customwere separated by filtration
  3. washwashed with chilled diethyl ether
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-8b9f424fc9d4433eb20ab9d86fad4cb7
出典データセット
uspto-grants-2005_06
特許番号
US06903107B1

関連ノート

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