Bromine → HCID 15511794, compound

Participants

Reaction Steps

A solution of 0.15 g (3.57 mmol) of lithium hydroxide hydrate in 10 mL of water was added to a solution of 0.6 g (0.903 mmol) of trans-3-{1-[2-(4-amino-3,5-dibromobenzoyl)cyclopropanecarbonyl]-4-piperidinyl}-3,4-dihydro-6-(methoxycarbonylmethoxy)-2(1H)-quinazolinone (Item No. 22) in a mixture of 10 mL of THF and 10 mL of methanol. After stirring for 14 hours at ambient temperature, the organic solvents were distilled off in vacuo and the residue remaining was combined with 3.6 mL of 1N hydrochloric acid. The precipitate formed was suction filtered and dried in vacuo at 30° C. The residue was taken up in tetrahydrofuran, the solution formed was filtered while hot and, after cooling, combined with diisopropyl ether until the precipitation reaction had ended. The precipitate was suction filtered. After drying in a circulating air drier 0.25 g (43% of theoretical) of colorless crystals were obtained. Rf 0.63 (MP C); IR (KBr): 1730 cm−1 (C═O); MS: ESI: (M−H+2Na)+=693/695/697 (Br2); (M−H)−: 647/649/651 (Br2); (M+Na)+: 671/673/675 (Br2).

Provenance & Evidence