反应详情

A solution of a thiosemicarbazide (10 mmol, 0.91 g) and 3,4-dichlorophenylacetyl bromide (10 mmol, 2.68 g) in dioxane (20 mL) was stirred at room temperature for 16 h. The precipitate of hydrobromide salt was filtered and washed with dioxane (3×10 mL) basified with 2N Na2CO3 (20 mL). The product was filtered, washed with water and dried (2.08 g, 80%). The product was generally satisfactory for further reaction. 1H NMR (400 MHz) δ 8.67 (s, 1H, NH), 8.00 (d, J=1.6 Hz, 1H), 7.76 (dd, J=1.6 Hz, J=8.4 Hz, 1H), 7.60 (d, J=8.4 Hz, 1H), 7.31 (s), 1H MS+(APCI), 259.68, (M+1; calcd 258.97 (M+)

1. filtrationThe precipitate of hydrobromide salt was filtered
2. washwashed with dioxane (3×10 mL)
3. filtrationThe product was filtered
4. washwashed with water
5. customdried (2.08 g, 80%)
6. customThe product was generally satisfactory for further reaction