Phosphorus oxychloride → HCID 22313247, compound

A mixture of 2-amino-5-(2-methoxyethyl)-6-methylpyrimidine-4-ol (600 mg, 3.27 mmol) and phosphorus oxychloride (6 ml) was kept at 90° C. for 5.5 hours. The reaction mixture was concentrated in vacuo. was added to the residue and an aqueous ammonia solution was cautiously added. The mixture was extracted with chloroform and the organic layer was washed with saturated brine, dried over sodium sulfate and the solvent was concentrated. The residue was purified by silica gel column chromatography (chloroform:ethyl acetate=8:2) to give the object compound (200 mg, 30.3%).

1. concentrationThe reaction mixture was concentrated in vacuo
2. additionwas added to the residue
3. additionan aqueous ammonia solution was cautiously added
4. extractionThe mixture was extracted with chloroform
5. washthe organic layer was washed with saturated brine
6. dry with materialdried over sodium sulfate
7. concentrationthe solvent was concentrated
8. customThe residue was purified by silica gel column chromatography (chloroform:ethyl acetate=8:2)

ORD record

ord-8b6d01f0f0b14c2a89a7ab50e184df1c

Source dataset

uspto-grants-2005_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06951866B2