Diethyl Ether → HCID 10221341, compound

Participants

Reaction Steps

##STR6## 30.8 g (0.1 mol) of N-acetyltrimetazidine, 600 ml of diethyl ether and 11.1 g (0.3 mol) of LiAlH4 are heated to and then maintained at reflux for 24 hours with vigorous stirring, the mixture is subsequently allowed to return to room temperature, and stirring is continued for a further 12 hours, after which the mixture is hydrolysed in succession with 10 ml of water, 10 ml of 4N sodium hydroxide solution and finally 30 ml of water. The mixture is filtered and the residue is washed three times with 200 ml of diethyl ether each time. The ethereal phases are removed and the residue is then taken up three times with 300 ml of CH2C2 each time. The organic phase obtained after filtration is dried over magnesium sulphate, and the solvent is then removed by evaporation in vacuo. The residue (approximately 20 g) is filtered over 150 g of silica using a mixture of chloroform and ethanol (97.5% -2.5%) as eluants. 18 g of N-ethyl-N'-(2-hydroxy-3,4-dimethoxybenzyl)-piperazine are obtained directly (yield: 64%).

Provenance & Evidence