HRID1902467

反应详情

EQUATION

反应方程式

HRID 1902467 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-(3,4,5-trimethoxyphenyl)-4-methyl-5-acetylthiazole (3.7 g corresponding to its 0.012 mol) was dissolved into 50 ml of ethanol, and 32 ml of an aqueous 2% solution of sodium hydroxide (0.013 mol) and 1.8 g (0.016 mol) of semicarbazide hydrochloride were added to the solution. The whole mixture was then heated for 5 hours under a reflux condenser. After cooling the reaction mixture to room temperature, the mixture was introduced into one liter of iced water. The precipitate which separated was collected by filtration, washed with water and was recrystallized from ethanol to obtain the object consisting of yellow needle-like crystals amounting to 3.0 g and melting at 240° to 242° C. The yield was 69%.

WORKUP

后处理

  1. additionwere added to the solution
  2. temperatureThe whole mixture was then heated for 5 hours under a reflux condenser
  3. customThe precipitate which separated
  4. filtrationwas collected by filtration
  5. washwashed with water
  6. customwas recrystallized from ethanol
  7. customto obtain the object