反应详情

A solution of carbon disulphide (4.2 g) in dry acetone (8 ml) was added dropwise to a solution of 5-[[(2-aminoethyl)thio]methyl]-N,N-dimethyl-2-furanmethanamine (10.71 g) in dry acetone (30 ml) during 15 minutes at -10° to 0°. To the stirred solution at -15° was added dropwise a solution of mercuric chloride (13.6 g) in dry acetone (20 ml) during 45 minutes. The solution was warmed to 0° and triethylamine (11.5 g) was added dropwise with stirring during 15 minutes. The mixture was refluxed for 45 minutes, the suspension filtered and the filtrate evaporated to dryness. The oily residue was dissolved in ether (150 ml), decolourising charcoal and excess anhydrous sodium sulphate were added and the suspension filtered after 2 hours. The filtrate was evaporated to dryness, the oily residue dissolved in ether and the solution chromatographed (alumina deactivated with water, 72.5 ml/kg/ether). The appropriate eluate was evaporated to give the title compound (5.05 g) as a brown oil.

1. temperatureThe solution was warmed to 0°
2. temperatureThe mixture was refluxed for 45 minutes
3. filtrationthe suspension filtered
4. customthe filtrate evaporated to dryness
5. dissolutionThe oily residue was dissolved in ether (150 ml)
6. additionwere added
7. filtrationthe suspension filtered after 2 hours
8. customThe filtrate was evaporated to dryness
9. dissolutionthe oily residue dissolved in ether
10. customthe solution chromatographed (alumina deactivated with water, 72.5 ml/kg/ether)
11. customThe appropriate eluate was evaporated