Lithium Hydroxide → HCID 21109742, compound

Participants

Reaction Steps

A solution of 0.24 g (10.0 mmol) of lithium hydroxide in 20 ml of water was added to a solution of 1.2 g (2.6 mmol) of (E)-3,4-dihydro-3-{1-[1,4-dioxo-4-(4-ethoxycarbonylphenyl)-2-buten-1-yl]-4-piperidinyl}-2(1H)-quinazolinone (Item no. 169) in 20 ml of THF. After stirring for 4 hours at ambient temperature the mixture was diluted with 200 ml of water and extracted once with 100 ml of tert.butylmethylether. The aqueous phase was acidified with 1N hydrochloric acid and extracted five times with a mixture of dichloromethane and methanol (9/1 v/v). The combined organic extracts were dried over sodium sulphate and concentrated by evaporation in vacuo. The residue remaining was triturated with diethylether and suction filtered. After drying in a circulating air dryer 0.5 g (44% of theoretical) of colourless crystals were obtained. Rf 0.72 (EE/MeOH/AcOH 80/20/5 v/v/v) or 0.43 (El D). IR (KBr): 1689 (C═O) MS: no M+

Provenance & Evidence