Diethyl Ether → 2,5-Dichloro-4-methoxypyrimidine

Temperature

0 °C

To a 250 mL round bottom flask equipped with a stir bar was added 2,4,5-trichloro-pyrimidine (1 g), and diethyl ether (15 mL). The mixture was cooled to 0° C. in an ice bath and then 1 equivalent of sodium methoxide in methanol (prepared from reacting 120 mg of sodium with 4 mL of methanol at room temperature) was slowly added. The reaction was stirred over night at room temperature and checked by LCMS. The white precipitate was filtered and the solid washed with cold methanol. After drying, 0.98 g of pure 2,5-dichloro-4-methoxypyrimidine was obtained and this material was used without further purification. 1H-NMR (DMSO): δ 8.61 (s, 1H), 4.05 (s, 3H).

1. customTo a 250 mL round bottom flask equipped with a stir bar
2. filtrationThe white precipitate was filtered
3. washthe solid washed with cold methanol
4. customAfter drying

ORD record

ord-af31d1a49a5245ad9e9fa11888135c1d

Source dataset

uspto-grants-2014_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08815882B2