反应详情

温度

110 °C

Into a two liter reactor, fitted with an oil-bath and stirring means and under nitrogen circulation, were poured 201.5 g (1 mol) of 5-(2-chloroethyl)-4,5,6,7-tetrahydro-thieno-(3,2-c)-pyridine and slowly, under stirring, 181 g (1 mol) of 3,4-dimethoxyphenethylamine. The reacting mixture was warmed at 110° C. under stirring for two hours. The oily mixture obtained was cooled to about 70°-80° C. and then poured into icy water; after separation, washing, extraction with diethyl ether and drying, the residue was dissolved in a mixture of petroleum ether and isopropyl ether (50/50 by volume) and passed through a silica gel column. Elution was with acetone. The fraction containing the desired compound was evaporated to dryness, treated with diethyl ether and finally with acetone. Yield 163 g (47%) of a white crystalline powder soluble in water, melting at 260° C. (Tottoli) with decomposition, the analysis and NMR of which showed a good correspondence with the formula C19H26N2O2S.

1. customInto a two liter reactor, fitted with an oil-bath
2. stirringslowly, under stirring
3. stirringunder stirring for two hours
4. customThe oily mixture obtained
5. temperaturewas cooled to about 70°-80° C.
6. customafter separation
7. washwashing
8. extractionextraction with diethyl ether
9. customdrying
10. dissolutionthe residue was dissolved in a mixture of petroleum ether and isopropyl ether (50/50 by volume)
11. washElution
12. additionThe fraction containing the desired compound
13. customwas evaporated to dryness
14. additiontreated with diethyl ether and finally with acetone