反应详情

Thiosemicarbazide (6.4 g, 70 mmol) was added under nitrogen to a solution of 4-chloro-4'-methoxybutyrophenone (10.0 g, 47 mmol) in 150 mL of methanol plus 12.7 mL of 1 N HCl plus 11.8 mL of water and the reaction stirred for approximately three days (over the weekend). The solid formed was collected by filtration and dissolved in methylene chloride. The organic solution was washed multiple times with water, dried (MgSO4) and the solvent removed under reduced pressure to give a white solid. Recrystallization of the solid from isopropyl alcohol gave 8.46 g (63%) of the title compound as a light yellow solid, mp 137-140° C.

1. customThe solid formed
2. filtrationwas collected by filtration
3. dissolutiondissolved in methylene chloride
4. washThe organic solution was washed multiple times with water
5. dry with materialdried (MgSO4)
6. customthe solvent removed under reduced pressure
7. customto give a white solid
8. customRecrystallization of the solid from isopropyl alcohol