HRID874942

反应详情

EQUATION

反应方程式

HRID 874942 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A suspension of 2-bromoacetophenone (5 g, 0.0251 mol), potassium thiocyanate (8.6 g, 0.088 mol) and potassium iodide (0.25 g, 0.0015 mol) in dry DMF (25 mL) was heated to 80° C. for 2 h. The reaction mixture was concentrated to dryness under reduced pressure and the residue was dissolved in glacial acetic acid (25 mL) and 50% aqueous H2SO4 was added to it. The reaction mixture was heated to 100° C. for 10 min. The reaction mixture was poured in ice water and the precipitate formed was filtered and dried under reduced pressure to get 4-phenylthiazol-2(3H)-one (3.3 g, yield 75%) as brown solid, which was carried through without further purification.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated to dryness under reduced pressure
  2. dissolutionthe residue was dissolved in glacial acetic acid (25 mL)
  3. addition50% aqueous H2SO4 was added to it
  4. temperatureThe reaction mixture was heated to 100° C. for 10 min
  5. additionThe reaction mixture was poured in ice water
  6. customthe precipitate formed
  7. filtrationwas filtered
  8. customdried under reduced pressure