反应 #692056

反应方程式

2,4′-dichloroacetophenone

potassium rhodanide

→

1-(4-chloro-phenyl)-2-thiocyanato-ethanone

收率 90.0%

反应条件

后处理

1. 1
   温度to reflux for 30 minutes
2. 2
   其他After a few minutes a precipitation
3. 3
   其他was formed
4. 4
   其他The solvent was evaporated under reduced pressure
5. 5
   过滤filtered
6. 6
   浓缩the filtrate was concentrated in vacuo
7. 7
   workup.STIRRINGThe residue was stirred with heptane and little ethanol for 15 minutes
8. 8
   过滤The product was filtered off
9. 9
   其他dried

实验过程

A solution of 945 mg (5 mmol) 2,4′-dichloroacetophenone and 583 mg (6 mmol) potassium rhodanide was heated to reflux for 30 minutes. After a few minutes a precipitation was formed. The solvent was evaporated under reduced pressure and the residue was suspended in tetrahydrofurane, stirred for 1 hour at room temperature, filtered and the filtrate was concentrated in vacuo. The residue was stirred with heptane and little ethanol for 15 minutes. The product was filtered off and dried to yield 953 mg (90%) 1-(4-chloro-phenyl)-2-thiocyanato-ethanone as a light yellow solid. 1H NMR (CDCl3, 250 MHz): δ (ppm)=7.89 (d, 2H), 7.51 (d, 2H), 4.692 (s, 2H).

来源