反应详情

Thiourea (0.29 g) and 4,4-difluorobut-3-enyl 4-methyl-benzenesulfonate (1 g) were heated together under reflux in ethanol (20 cm3) for 24 hours. The reaction mixture was cooled and the solvent evaporated under reduced pressure to give an oil which slowly crystallised. Trituration with hexane gave (4,4-difluorobut-3-enyl)-thiourea as its 4-methyl-benzenesulfonate salt (1.14 g). MH+ (FAB)=167; 1H NMR (DMSO-d6): δ 2.48(3H,s); 2.46-2.58(2H,m); 3.42(2H,t); 4.66-4.84(1H,m); 7.32(2H,d); 7.68(2H,d); 9.10-9.40(3H,br).

1. temperatureThe reaction mixture was cooled
2. customthe solvent evaporated under reduced pressure
3. customto give an oil which
4. customslowly crystallised