Sodium Sulfite → HCID 88580856, compound

Temperature

2.5 °C

Combine 6-chloro-2-methylpyrimidin-4-amine (708 g, 4.93 mol) and MeOH (7.08 L) in a 20 L round bottom flask equipped with a mechanical stirrer. Cool to 0-5° C. Add iodine monochloride (4.806 kg, 29.6 mol) dissolved in MeOH (6 L) using an addition funnel over a period of 1 h. Warm the reaction mixture to RT and stir at RT for 16 h. Cool the reaction mixture to 0-5° C. and add sodium sulfite (46 L, 20% aqueous solution). Filter the resulting solid and wash with water (2 L) followed by hexane (3 L). Dry the solid under vacuum to afford the title compound as a white solid (1061 g, 80%). LC-ES/MS m/z 269.9 (M+1).

1. customof 1 h
2. temperatureWarm the reaction mixture to RT
3. temperatureCool the reaction mixture to 0-5° C.
4. filtrationFilter the resulting solid
5. washwash with water (2 L)
6. customDry the solid under vacuum

ORD record

ord-f70f3c19650644a99b8c0b25040f25f2

Source dataset

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09035051B1