Water → HCID 21956060, Verbindung

4-amino-6-chloro-2-(4-fluorophenyl)-5-nitropyrimidine (15.3 g, 57 mmol) was dissolved in a mixture of methanol (200 mL) and ethyl acetate (100 mL), and after adding thereto 10% palladium on carbon (2.88 g) and triethylamine (12 mL), the mixture was stirred in a hydrogen stream for 18 hours. The reaction mixture was filtered and the filtrate was concentrated in vacuo to give a residue, to which was added water. The mixture was extracted with ethyl acetate, and the organic layer was dried over anhydrous magnesium sulfate, then concentrated in vacuo. The residue was purified by silica gel column chromatography (C-300, chloroform:methanol=20:1) to give the title compound as a brown solid (7.16 g, 68%).

1. additionafter adding
2. filtrationThe reaction mixture was filtered
3. concentrationthe filtrate was concentrated in vacuo
4. customto give a residue
5. extractionThe mixture was extracted with ethyl acetate
6. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
7. concentrationconcentrated in vacuo
8. customThe residue was purified by silica gel column chromatography (C-300, chloroform:methanol=20:1)

ORD-Eintrag

ord-7df2f4206b784d49913c738df693f028

Quelldatensatz

uspto-grants-2010_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07803807B2