HRID1172228

反应详情

EQUATION

反应方程式

HRID 1172228 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 20 mL of absolute ethanol, 250 mg of metallic sodium was added in small portions. After dissolved completely, 760 mg of thiourea was added to the above solution, and the mixture was stirred at room temperature for 1 hour. To the reaction, 2.11 g of N-[4-(2,2-dicyanovinyl)phenyl]acetamide was added, and the mixture was heated to reflux for 3 hours. Then, the solvent was removed under reduced pressure from the reaction mixture, the residue was dissolved in 30 mL of water. In addition, the mixture was acidified by adding acetic acid in small portions, thereto 30 mL of ethyl acetate was added and then the solution was stirred overnight. Filtration of the precipitated material gave 1.2 g of N-[4-(6-amino-5-cyano-2-mercapto-2,3-dihydropyrimidin-4-yl)phenyl]acetamide as a white powder.

WORKUP

后处理

  1. dissolutionAfter dissolved completely
  2. additionwas added
  3. temperaturethe mixture was heated
  4. temperatureto reflux for 3 hours
  5. customThen, the solvent was removed under reduced pressure from the reaction mixture
  6. dissolutionthe residue was dissolved in 30 mL of water
  7. additionby adding acetic acid in small portions
  8. addition30 mL of ethyl acetate was added
  9. stirringthe solution was stirred overnight
  10. filtrationFiltration of the precipitated material