Hydrochloric Acid → 2,4-Dichloro-6-methyl-1,3,5-triazine

Temperature

10 °C

In a 2 l flask equipped with a mechanical stirrer, a dry ice condenser, a thermometer and a gas inlet was charged 700 ml of toluene and 50 g of N-methylacetamide. It was cooled to 10° C. and then was charged 60 g of phosgene at 10°-20° C. Afterwards, 30 g of HCl gas was introduced. Then, 50 g of sodium dicyanamide was charged in one portion and the HCl charge continued until 56 g of total HCl was introduced. The reaction mass was heated to 65° C. for 2 hours. After cooling to 20° C., the reaction content consisted of toluene and some tars. The toluene phase was decanted into 500 ml of ice water. The residue was rinsed with 300 ml of toluene and then decanted. The combined toluenes were washed with water (2×500 ml) and dried over MgSO4. After evaporation, 32.5 g of 2,4-dichloro-6-methyl-1,3,5-triazine was obtained as white needles (35% yield).

1. customIn a 2 l flask equipped with a mechanical stirrer, a dry ice condenser
2. additionwas introduced
3. temperatureThe reaction mass was heated to 65° C. for 2 hours
4. temperatureAfter cooling to 20° C.
5. customthe reaction
6. customThe toluene phase was decanted into 500 ml of ice water
7. washThe residue was rinsed with 300 ml of toluene
8. customdecanted
9. washThe combined toluenes were washed with water (2×500 ml)
10. dry with materialdried over MgSO4
11. customAfter evaporation

ORD record

ord-e9c2480114284139b73a9af73d5e0ab7

Source dataset

uspto-grants-1992_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05095113