반응 #2467934

반응 방정식

thiosemicarbazide

3,4-dichlorophenylacetyl bromide

→

4-(3,4-Dichloro-phenyl)-thiazol-2-yl-hydrazine

용매

dioxane

반응 조건

후처리

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

실험 절차

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+)

출처