3-Methoxypropylamine → HCID 57625429、化合物

反応式

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

参加物

反応物 2

HCID 16723-Methoxypropylamine

HCID 12015126-chloropyridine-3-sulfonamide

生成物 1

HCID 57625429HCID 57625429、化合物収率 78%

反応条件

温度: 100 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード: ord-084babfdb0394ccc982d4da7d95862cf
出典データセット: uspto-grants-2011_12
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08071597B2

反応ノート

読み込み中…

参加物