Dimethyl Sulfide → HCID 13363100, compound

Temperature

-20 °C

To a solution of 15.5 g (0.10 mole) of 2-amino-4,6-dimethoxypyrimidine and 8 ml (0.109 mole) of methylsulfide in 100 ml of methylene chloride at -20° C. was added dropwise a solution of 13.3 g (0.10 mole) of N-chlorosuccinimide in 300 ml of methylene chloride. After addition, the resulting solution stirred at -20° C. for 2 hours and then warmed up to room temperature. The solution was stirred at room temperature for another hour. The solution was washed with 400 ml of 2.5% sodium hydroxide aqueous solution and then 400 ml of water. The organic layer was separated, dried over sodium sulfate and concentrated under reduced pressure. The residue was washed with ethyl ether, and dried under vacuum at ambient temperature to afford 6 g of the title compound as a solid, m.p. 102°-103° C. (dec.).

1. additionAfter addition
2. temperaturewarmed up to room temperature
3. stirringThe solution was stirred at room temperature for another hour
4. washThe solution was washed with 400 ml of 2.5% sodium hydroxide aqueous solution
5. customThe organic layer was separated
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated under reduced pressure
8. washThe residue was washed with ethyl ether
9. customdried under vacuum at ambient temperature

ORD record

ord-86ad0fdca08941c7b2d9665463975fc9

Source dataset

uspto-grants-1986_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04604133