Dimethyl Sulfate → hexahydro-3-(3-methoxyphenyl)-1-methyl-2H-azepin-2-one

Participants

Reaction Steps

Hexahydro-3-(3-hydroxyphenyl)-1-methyl-2H-azepin-2-one (21.9 g) was dissolved in 2 M sodium hydroxide solution (100 ml) and dimethyl sulphate (18.3 g, 14.5 ml) added. The reaction mixture was stirred at room temperature for 10 minutes then seeded. The product crystallised after leaving at 0° C. for 3 hours. The product was filtered, washed with water and dried affording 16.99 g of title compound as off-white powder m.p. 73°-74° C., identical to that obtained in Example 2.

Provenance & Evidence