Reaktion #65154
ord-88506e12a7c6447fb7f6d563c2d9e044
Reaktionsgleichung
Edukte
Reagenzien
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Trocknendried over anhydrous sodium sulfate
- 2FiltrationThe mixture was filtered through a small amount of silica gel
- 3Einengenthe filtrate was concentrated in vacuo
Vorschrift
3-Chloropropylsulfonyl chloride 1 (6.8 g,94.9 mmol), methylamine hydrochloride (13.5 g,200 mmol), and potassium carbonate (27.6 g,200 mmol) were added in turn to ethyl acetate (500 ml). After the addition of N-benzyltrimethylammonium chloride (about 200 mg), the resultant mixture was stirred for 2 hours at room temperature and dried over anhydrous sodium sulfate. The mixture was filtered through a small amount of silica gel and the filtrate was concentrated in vacuo to give 12 g (74%) of crude N-methyl-3-chloropropylsulfonamide (intermediate 3b) as a pale yellow oil.