3-Methoxypropylamine → HCID 57625429, 화합물

반응식

Cl[C:2]1[N:7]=[CH:6][C:5]([S:8]([NH2:11])(=[O:10])=[O:9])=[CH:4][CH:3]=1.[CH3:12][O:13][CH2:14][CH2:15][CH2:16][NH2:17]>>[CH3:12][O:13][CH2:14][CH2:15][CH2:16][NH:17][C:2]1[N:7]=[CH:6][C:5]([S:8]([NH2:11])(=[O:10])=[O:9])=[CH:4][CH:3]=1

참가 물질

반응물 2

HCID 16723-Methoxypropylamine

HCID 12015126-chloropyridine-3-sulfonamide

생성물 1

HCID 57625429HCID 57625429, 화합물수율 78%

반응 조건

온도: 100 °C

실험 절차

A mixture of 6-chloropyridine-3-sulfonamide (5 g, 0.025 mol) and 3-methoxy propylamine (50 ml) is stirred at 100° C. for 12 h. The mixture is cooled and excess reagent is removed by distillation. The residue is suspended in DCM (25 ml) and cooled. The precipitate is filtered, washed with cold ammonium hydroxide (2×50 ml) and dried under vacuum to afford 5 g (78%) of the titled compound as a white solid. mp: 129-132° C., LC/MS: (ES+) 246.

후처리

temperatureThe mixture is cooled
customexcess reagent is removed by distillation
temperaturecooled
filtrationThe precipitate is filtered
washwashed with cold ammonium hydroxide (2×50 ml)
customdried under vacuum

출처 및 근거

ORD 기록: ord-73a9e1dce66240e7ae895d8f06b89d00
출처 데이터셋: uspto-grants-2014_11
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08877757B2

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