反应详情

6 ml of tetrahydrofuran (THF) and 3.5 mmol of 1-benzyl-4-(1-phenyl-2,2-dimethoxyethylamino)-(S,S)-3,5-bis(1-methoxyethyl)-1,2,4-triazolium bromide are introduced into a 100 ml round-bottomed flask equipped with a reflux condenser and a magnetic stirrer and then 1.75 ml of a 2 mol/l solution of lithium borohydride in THF are added at ambient temperature over a period of 1 to 2 h approximately. The reaction medium is subsequently left stirring at ambient temperature for 3 h and then brought to reflux for 3 h. After returning to ambient temperature, 20 ml of a 20% aqueous sodium hydroxide solution are added and then the aqueous phase is extracted with dichloromethane. The resulting organic phase is dried over anhydrous magnesium sulphate and then concentrated. The amine is purified by distillation. 0.19 g of the expected compound is obtained.

1. customequipped with a reflux condenser and a magnetic stirrer
2. waitThe reaction medium is subsequently left
3. temperatureto reflux for 3 h
4. customAfter returning to ambient temperature
5. extractionthe aqueous phase is extracted with dichloromethane
6. dry with materialThe resulting organic phase is dried over anhydrous magnesium sulphate
7. concentrationconcentrated
8. distillationThe amine is purified by distillation