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ChemicalBook CAS DataBase List (R)-2-chloro-7-ethyl-8-isopropyl-7,8-dihydropteridin-6(5H)-one

(R)-2-chloro-7-ethyl-8-isopropyl-7,8-dihydropteridin-6(5H)-one synthesis

4synthesis methods
-

Yield:889877-77-4 90%

Reaction Conditions:

Stage #1: methyl (2R)-2-[(2-chloro-5-nitropyrimidin-4-yl)(propan-2-yl)amino]butanoatewith hydrogen;platinum on carbon in tetrahydrofuran at 35; under 2250.23 Torr;
Stage #2: bis(acetylacetonate)oxovanadium in tetrahydrofuran;

Steps:

ii

50 g 23 in 375 mL of tetrahydrofurane is hydrogenated in the presence of 5 g Platinum on Carbon (5%) at a hydrogene pressure of 3 bar and at 35 °C until no further hydrogene consumed. 2.5 g vanadyl acetylacetonate are added and the hydrogenation is continued. The suspension is filtered to remove the catalysts. The solvent is removed under reduced pressure. 150 mL 2-propanol are added to the residue and heated to reflux. 300 ml of demineralised water are added. The suspension is cooled slowly to 2 °C. The suspension is suction filtered and washed with a cold mixture of 2- propanol and demineralised water. After drying in a vacuum drying oven at 50°C, 36 g (90% of theory) of product 24 is obtained

References:

WO2007/90844,2007,A1 Location in patent:Page/Page column 13