反应详情

A suspension of lithium aluminium chloride (8.2 g) in dry ether (170 ml) was treated dropwise with a solution of aluminium chloride (8.2 g) in ether (170 ml) under cooling. After stirring for half an hour at room temperature a solution of 1-(1,4-benzodioxan-5-yl)-4-cyanomethylpiperazine (9.4 g) in dry tetrahydrofuran (250 ml) was added dropwise at 15° C. After reflux for 1.5 h the mixture was cooled and conc. sodium hydroxide solution (40 ml) was added dropwise. Filtration and removal of solvent in vacuo gave an oil which was dissolved in methylene chloride and dried over magnesium sulfate. Removal of solvent in vacuo gave 1-(2-amino-1-ethyl)-4-(1,4-benzodioxan-5-yl)piperazine (9.1 g) as a viscous oil.

1. temperatureunder cooling
2. additionwas added dropwise at 15° C
3. temperatureAfter reflux for 1.5 h the mixture
4. temperaturewas cooled
5. filtrationFiltration and removal of solvent in vacuo
6. customgave an oil which
7. dry with materialdried over magnesium sulfate
8. customRemoval of solvent in vacuo