Dimethyl Sulfate → HCID 178463891, compound

Participants

Reaction Steps

500 cc of sodium hydroxide solution 1N are added while stirring to 91.5 g (0.5 mol) of 2-diethylamino-4,6-dihydroxy-pyrimidine. The solution is stirred at 50° for a short period and then cooled to 20° . 63 g (0.5 mol) of dimethyl sulphate are added dropwise, over the course of 1 hour, to the clear solution; by further addition of 1N sodium hydroxide solution the pH value is kept between 7.5 and 8. A total of approximately 100 cc of 1N sodium hydroxide solution is additionally required. The mixture is stirred for a further 5 hours at room temperature and the precipitated crystals are filtered off at 5°; then they are washed with water. The crystalline product is subsequently triturated with 1500 cc of carbon tetrachloride by means of a vibration mixer. The undissolved parts are suction filtered and the carbon tetrachloride solution is then concentrated by evaporation, whereupon crystallization commences; 200 cc of petroleum ether are then added.

Provenance & Evidence