Methyl iodide → HCID 178439474, compound

A 1N solution of potassium hydroxide in methanol (110 mL) was added dropwise at 0° C. to a suspension of 2-mercapto-6-propyl-pyrimidin-4-ol (17.0 g) in methanol (220 mL). The mixture was stirred at room temperature for 15 minutes. After cooling at 0° C., iodomethane (6.8 mL) was added dropwise over 15 minutes. The mixture was stirred at room temperature for 6 hours, then filtered. The first precipitate was successively washed with methanol, water, isopropanol, then dried under reduced pressure. The filtrate was concentrated under reduced pressure, triturated with water, filtered. The second precipitate was successively washed with methanol, water, isopropanol, then dried under reduced pressure. Both precipitates were combined to afford 2-methylsulfanyl-6-propyl-pyrimidin-4-ol (15.5 g) as white crystals (mp=158° C.).

1. temperatureAfter cooling at 0° C.
2. stirringThe mixture was stirred at room temperature for 6 hours
3. filtrationfiltered
4. washThe first precipitate was successively washed with methanol, water, isopropanol
5. customdried under reduced pressure
6. concentrationThe filtrate was concentrated under reduced pressure
7. customtriturated with water
8. filtrationfiltered
9. washThe second precipitate was successively washed with methanol, water, isopropanol
10. customdried under reduced pressure

ORD record

ord-f7aae4a0d68e4987b1a830249174e599

Source dataset

uspto-grants-2009_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07589095B2