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ChemicalBook CAS DataBase List Valacyclovir hydrochloride

Valacyclovir hydrochloride synthesis

5synthesis methods
-

Yield:124832-27-5 92%

Reaction Conditions:

with hydrogenchloride;5%-palladium/activated carbon;hydrogen in water at 25 - 30; under 2250.23 - 6000.6 Torr;Concentration;

Steps:

2

To a 1L capacity hydrogenator charged a compound of formula II (50g), concentrated hydrochloric acid (9.6ml), 5% palladium on carbon (5g) and water (350ml) and hydrogenate the reaction mass under hydrogen pressure of 3 kg/cm 2 to 8 kg/cm 2 at a temperature of 25-30°C for 6 to 12 hours. The reaction mass was filtered under vacuum and washed with water. The filtrate was then distilled off under vacuum. The reaction mass was then cooled and isopropyl alcohol was added to the reaction mass. The reaction mass was further cooled to a temperature of 5-10°C and maintained for 1 hour. The product valacyclovir hydrochloride obtained was filtered and washed with isopropyl alcohol.Yield 92% and purity 99.8%ANALYTICAL METHOD FOR ANALYSISHPLC column : USP LI, 4.6 x 150 mm, 3.5 ???(Zorbax SB-C18, Part No. 863953-914)Detector : UV 250nmMobile phase A : In a 1000ml volumetric flask add 2.8ml of triethylamine, 800ml of purified water and adjust the pH to 5.00 + 0.05 with glacial acetic acid. Complete the volume with purified water.Mobile Phase B AcetonitrileInjection volume 50??,Column temperature 30°CFlow rate l.OmL/minutesGradient

References:

WO2013/76688,2013,A1 Location in patent:Page/Page column 10-11

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