反应详情

A 5 g portion of the above aldehyde was dissolved in 100 ml of ethanol, cooled to 0°-5° C. and a solution of 2.14 g of ethylenediamine in 10 ml of ethanol was added dropwise with stirring. The mixture was allowed to come to room temperature over 3 hours, then 2.4 g of sodium borohydride was added and the mixture was stirred for 18 hours. Water was added, then the mixture was concentrated. The residue was dissolved in dichloromethane, cooled, extracted with water, dried, filtered and evaporated to an oil which crystallized, giving 4.6 g of 2-(3-methyl-2-thienyl)piperazine.

1. temperaturecooled to 0°-5° C.
2. stirringthe mixture was stirred for 18 hours
3. concentrationthe mixture was concentrated
4. dissolutionThe residue was dissolved in dichloromethane
5. temperaturecooled
6. extractionextracted with water
7. customdried
8. filtrationfiltered
9. customevaporated to an oil which
10. customcrystallized