3-Pentanol → HCID 58045802, compound

Participants

Reaction Conditions

Reaction Steps

3-Pentanol (20 ml) was initially charged under argon, admixed with sodium hydride (946 mg) and stirred at 50° C. for 1 h. Subsequently, 6-chloro-7,8,9,10-tetrahydro-[1,2,4]triazolo[3,4-a]-phthalazin-3-ylamine hydrobromide (W2.018, 1.88 g), dissolved in 3-pentanol (20 ml) and DMF (100 ml), was slowly added dropwise within 1 h. After stirring for 1 h, the mixture was concentrated, and the residue was admixed with water and extracted four times with dichloromethane. The combined organic phases were dried over magnesium sulfate, filtered and concentrated. The residue was purified using a 40 g silica gel cartridge (0-10% dichloromethane-methanol gradient in 50 min). The clean product fractions were combined and dried. 0.8 g of the title compound was obtained.

Provenance & Evidence