Water → HCID 21956060、化合物

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レコード

ord-914858cda731418996ca829c05b9d8bd

出典データセット

uspto-grants-2010_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07687514B2