反应详情

A mixture of 5-chloro-2-(methylamino)pyridine (0.41 g), 2-ethoxy-1,1-bis(phenylsulphonyl)ethene and concentrated hydrochloric acid (1 drop) in toluene (20 ml) was heated at reflux for 4 hours and then the mixture was treated with 1,5-diazabicyclo[4.3.0]-non-5-ene (3 drops) and heated at reflux for 18 hours. The reaction mixture was cooled and concentrated in vacuo to give an oil which was triturated with ethanol to give a brown solid which was recrystallised from toluene to give 1,1-bis(phenylsulphonyl)-2-[N-(5-chloropyrid-2-yl)-N-methylamino]ethene (0.2 g), mp. 205°-206° C.

1. temperaturewas heated
2. temperatureat reflux for 4 hours
3. temperatureheated
4. temperatureat reflux for 18 hours
5. temperatureThe reaction mixture was cooled
6. concentrationconcentrated in vacuo
7. customto give an oil which
8. customwas triturated with ethanol
9. customto give a brown solid which
10. customwas recrystallised from toluene