HRID1679244

反应详情

EQUATION

反应方程式

HRID 1679244 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Sodium carbonate (1.06g. 0.010 mole) was dissolved in water (100 ml). Bis(carboxymethyl)trithiocarbonate (4.52g, 0.02 mole) was added portionwise with vigorous stirring. When solution was complete, the reaction mixture was warmed to 80°-85° C and 1-acetyl-2-(4-aminophenyl)hydrazine (3.30 g, 0.020 moles) was added in one portion. The reaction mixture was heated with stirring for 11/2 hours, cooled to about 50°-60° C, then reheated at 80°-85° C. The product began to precipitate during reheating. After another 2 hours of heating the mixture was cooled to room temperature, chilled and filtered. The solid which was collected was washed with water and dried. Yield 2.95g (53%), mp 210°-213° C (dec).

WORKUP

后处理

  1. temperaturethe reaction mixture was warmed to 80°-85° C
  2. temperatureThe reaction mixture was heated
  3. temperaturecooled to about 50°-60° C
  4. customreheated at 80°-85° C
  5. customto precipitate
  6. temperatureAfter another 2 hours of heating the mixture
  7. temperaturechilled
  8. filtrationfiltered
  9. customThe solid which was collected
  10. washwas washed with water
  11. customdried