HRID604874

反应详情

EQUATION

反应方程式

HRID 604874 的结构方程式

PROCEDURE

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).

WORKUP

后处理

  1. temperatureto reflux for 30 minutes
  2. customAfter a few minutes a precipitation
  3. customwas formed
  4. customThe solvent was evaporated under reduced pressure
  5. filtrationfiltered
  6. concentrationthe filtrate was concentrated in vacuo
  7. stirringThe residue was stirred with heptane and little ethanol for 15 minutes
  8. filtrationThe product was filtered off
  9. customdried