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

HRID 2304295노트

반응식

HRID 2304295 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 226656837-Methoxy-isoquinoline-N-oxide hydrochloride

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회HCID 6344Dichloromethane용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-f308ad24ba88412fb0a54642d20b8490
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06432955B1

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