Piperidine → Piperidine-1-sulfonyl chloride
反応式
[S:1]([Cl:5])(Cl)(=[O:3])=[O:2].[NH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1>>[N:6]1([S:1]([Cl:5])(=[O:3])=[O:2])[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1参加物
3
反応条件
- 温度
- 0 °C
実験手順
A solution of sulfuryl chloride (1N in dichloromethane, 75 mL, 75 mmol) at −20° C. was treated dropwise with piperidine (12.6 g, 150 mmol), stirred at 0° C. for 2 hours, and partitioned between dichloromethane and water (50 mL). The organic layer was washed with aqueous 1N HCl, brine and dried over anhydrous magnesium sulfate, filtered, and concentrated under reduced pressure. The residue was distilled under reduced pressure (1 mm Hg) at 105° C. to give the title compound (5 grams).
後処理
- custompartitioned between dichloromethane and water (50 mL)
- washThe organic layer was washed with aqueous 1N HCl, brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- concentrationconcentrated under reduced pressure
- distillationThe residue was distilled under reduced pressure (1 mm Hg) at 105° C.
出典と根拠
- ORDレコード
- ord-42a00bc52f6140398ccdc6b6f995e306
- 出典データセット
- uspto-grants-2011_03
- 特許番号
- US07902203B2
反応ノート
読み込み中…