反应详情

A mixture of 2.02 g (10.0 mmol) of 2-nitrobenzene-sulfonamide, 1.46 g (10.0 mmol) of dimethyl N-cyanodithioiminocarbonate and 1.38 g (10.0 mmol) of powdered, anydrous K2CO3 in 16 ml of acetone was heated at reflux for 20 hours. The reaction mixture was filtered and the solid collected was washed several times with acetone. The filtrate was evaporated and the orange oily residue was triturated with ether to afford a solid. The solid was collected by filtration, washed with ether and suspended in 10 ml of IN HCl. After stirring for 1 hour the solid was collected by filtration, washed with water and dried to yield 1.65 g (55 percent) of the desired product as a cream colored solid, mp 122° C. (decomposition). IR and 1H NMR spectra were consistent with the assigned structure.

1. temperatureat reflux for 20 hours
2. filtrationThe reaction mixture was filtered
3. customthe solid collected
4. washwas washed several times with acetone
5. customThe filtrate was evaporated
6. customthe orange oily residue was triturated with ether
7. customto afford a solid
8. filtrationThe solid was collected by filtration
9. washwashed with ether
10. filtrationwas collected by filtration
11. washwashed with water
12. customdried