Methanol → 2-Chloro-4,6-dimethoxy-1,3,5-triazine

Participants

Reaction Conditions

Reaction Steps

In a 500-ml four-necked flask equipped with a stirrer and a thermometer, 44.1 g (0.525 mol) of sodium hydrogencarbonate and 160.2 g (water content: 650 ppm, 5.0 mol) of methanol were placed. With stirring at a temperature of not higher than 10° C., 46.1 g (0.25 mol) of cyanuric chloride was added, followed by stirring at 20° C. for 1 hour. Then, the reaction was conducted at 60° C. for 3.5 hours. The weight of the reaction solution from which a salt formed had been removed was 192 g, and the water content was 49,500 ppm. After cooling, methanol was distilled off. To the residue, 200 ml of water was added, and the objective product was extracted with 250 ml of ethyl acetate. The organic layer was washed with 100 ml of water and then vacuum concentrated to obtain 39.2 g of 2-chloro-4,6-dimethoxy-1,3,5-triazine as a white solid. The yield was 89.2%. From the gas chromatography analysis, the purity proved to be 96.3% (% by area).

Provenance & Evidence