反应详情

温度

100 °C

500 mg (2.16 mmol) 5′-amino-3-methyl-1′,3′-dihydrospiro[imidazolidine-4,2′-indene]-2,5-dione (Bioorg. Med. Chem. Lett.; 2006; 16; 24; 6165-6169) and 400 μL (2.33 mmol) DIPEA were added to 400 mg (2.14 mmol) ethyl 6-chloropyrimidine-4-carboxylate in 10 mL DMF and the reaction mixture was stirred for 8 h at 100° C. The reaction mixture was diluted with 60 mL water and stirred for 30 min. The precipitate was suction filtered and the filtrate was extracted with dichloromethane (3×40 mL). The organic phases were combined, dried on magnesium sulphate, filtered and evaporated down i.vac. The residue was dissolved in DMF and purified by preparative HPLC. The product fractions were combined and freeze-dried.

1. stirringstirred for 30 min
2. filtrationfiltered
3. extractionthe filtrate was extracted with dichloromethane (3×40 mL)
4. customdried on magnesium sulphate
5. filtrationfiltered
6. customevaporated down i.vac
7. dissolutionThe residue was dissolved in DMF
8. custompurified by preparative HPLC
9. customfreeze-dried