Hexane → 1245830-98-1

To a solution of 2,4,5-trichloropyrimidine (5 g, 27.32 mmol) in THF:water (1:1, 40 mL), was added sodium thiomethoxide (2.15 g, 30.01 mmol) at 0° C., and the mixture was stirred at rt for 4 h. TLC showed completion of starting material and formation of a slightly polar spot (TLC system: hexane charred in iodine). The reaction mixture was concentrated, water (20 ml) was added, and the product was extracted with ethyl acetate (2×20 ml). The organic layer was dried over sodium sulfate and concentrated to afford the desired compound as a white solid (5 g, 94.8%). MS m/z: 195.2 (ES+, M+H).

1. concentrationThe reaction mixture was concentrated
2. additionwater (20 ml) was added
3. extractionthe product was extracted with ethyl acetate (2×20 ml)
4. dry with materialThe organic layer was dried over sodium sulfate
5. concentrationconcentrated

ORD record

ord-104623fcea224ed6af37325f88f6954c

Source dataset

uspto-grants-2015_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09145387B2