Piperidine → Piperidine-1-sulfonyl chloride
Reaktionsgleichung
[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]1Komponenten
3
Reaktionsbedingungen
- Temperatur
- 0 °C
Versuchsvorschrift
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).
Aufarbeitung
- 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.
Quellen und Nachweise
- ORD-Eintrag
- ord-42a00bc52f6140398ccdc6b6f995e306
- Quelldatensatz
- uspto-grants-2011_03
- Patentnummer
- US07902203B2
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