反应详情

Thiosemicarbazide (9.11 g, 0.1 mol) was added under nitrogen to a solution 4-chloro-2'-butyrothienone (16.2 mL, 0.1 mol) in 350 mL of methanol plus 27 mL 1N HCl plus 25 mL of water. After stirring at room temperature for approximately 2 hours, all of the solid had dissolved. The reaction was then stirred at room temperature for 24 hours (overnight). By TLC starting material remained. An additional 27 mL of 1N HCl was added and the reaction stirred at room temperature for 6 hours. The solid formed was removed by filtration and dried under high vacuum to give 14.87 g (57%) of the title compound as a brown solid, mp 120-122° C.

1. dissolutionall of the solid had dissolved
2. stirringThe reaction was then stirred at room temperature for 24 hours (overnight)
3. stirringthe reaction stirred at room temperature for 6 hours
4. customThe solid formed
5. customwas removed by filtration
6. customdried under high vacuum