Methyl iodide → HCID 90177069, compound

Temperature

50 °C

To a solution 6-bromopyrimidin-4(3H)-one (696 mg, 2.0 mmol) in DMF (3.0 mL) was added K2CO3 (828 mg, 6.0 mmol), CH3I (568 mg, 4.0 mmol), the reaction mixture was stirred at 50° C. for 30 minutes. The mixture was cooled to ambient temperature, diluted with EtOAc (20 mL), washed with sodium bicarbonate (10 mL) and brine (10 mL), dried over MgSO4, filtered and concentrated. The residue was purified with silica gel column (Petroleum ether:ethyl acetate=1:1) to obtain product: LC/MS m/z=189.01 (M+H)+.

1. temperatureThe mixture was cooled to ambient temperature
2. washwashed with sodium bicarbonate (10 mL) and brine (10 mL)
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified with silica gel column (Petroleum ether:ethyl acetate=1:1)
7. customto obtain product

ORD record

ord-581d3e5f743f4a88ab56a23fc669625c

Source dataset

uspto-grants-2016_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09273033B2