Chlorosulfonic acid → 4-(1-Acetylpiperidin-4-yl)benzenesulphonyl chloride
反応式
[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[Cl:16][S:17](O)(=[O:19])=[O:18]>>[C:1]([N:4]1[CH2:5][CH2:6][CH:7]([C:10]2[CH:15]=[CH:14][C:13]([S:17]([Cl:16])(=[O:19])=[O:18])=[CH:12][CH:11]=2)[CH2:8][CH2:9]1)(=[O:3])[CH3:2]参加物
3
実験手順
1-Acetyl-4-phenylpiperidine, [Chem. Abs., 75, 5728b (1971] (16.30 g) was added portionwise over 1 hour to stirred chlorosulphonic acid (53.3 ml) at 0°. The solution was stirred at 0° for 1 hour, then at room temperature for 2 hours, and then finally poured cautiously onto an excess of ice. When the ice had melted the mixture was extracted several times with dichloromethane. The combined organic extracts were washed with water, dried (Na2SO4) and evaporated to give the title compound, (23.0 g), m.p. 133°-134°, used directly in the next step.
後処理
- waitat room temperature for 2 hours
- additionfinally poured cautiously onto an excess of ice
- extractionwas extracted several times with dichloromethane
- washThe combined organic extracts were washed with water
- dry with materialdried (Na2SO4)
- customevaporated
出典と根拠
- ORDレコード
- ord-7758a8711e374a31a578e2d63a02b74d
- 出典データセット
- uspto-grants-1989_05
- 特許番号
- US04835165
反応ノート
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