Reaktion #55700

Reaktionsgleichung

N-methylcaprolactam

dimethylsulfate

→

2-methoxy-1-methyl-4,5,6,7-tetrahydro-3H-azepinium methylsulfate

Ausbeute 182.3%

Lösungsmittel

diethyl ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturCool
2. 2
   Sonstigethe resulting reaction mixture to ambient temperature

Vorschrift

Stir 190 g of N-methylcaprolactam and 189 g of dimethylsulfate for 3 hours at 80° C. Cool the resulting reaction mixture to ambient temperature before shaking it with diethyl ether and then freeing it from solvent residue in vacuo to obtain 346 grams (g) of 2-methoxy-1-methyl-4,5,6,7-tetrahydro-3H-azepinium methylsulfate as a light yellow oil. Add this oil, drop by drop, to a solution of 110 g of dimethylamine in 600 milliliters (ml) of benzene while stirring and boil the thus-prepared admixture under reflux for 90 minutes. Collect the heavy phase and extract it several times with diethyl ether. Concentrate the produced yellowish oil in vacuo to obtain 336 g (93% of theory) of the title compound.

Quelle