HRID1702847

反应详情

EQUATION

反应方程式

HRID 1702847 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Chloro-3-quinoxalinecarboxylic acid ethyl ester (7.10 g., 0.03 mole) was dissolved in 125 ml. of acetone treated with Norit and filtered. The filtrate was added to 5.650 g. (0.03 mole) of 1,3-di-n-butylthiourea in 100 ml. of acetone. The solution was stirred at reflux under a nitrogen atmosphere for 6 hours, allowed to cool to room temperature, and stirred an additional 17 hours. The red solution was treated with Norit, filtered, and concentrated to a volume of 100 ml. The yellow solid that crystallized out was collected by filtration, washed and dried to give the 6.05 g. (47.5% yield) of product, m.p. 138°-139° C. (dec.).

WORKUP

后处理

  1. filtrationfiltered
  2. additionThe filtrate was added to 5.650 g
  3. temperatureat reflux under a nitrogen atmosphere for 6 hours
  4. stirringstirred an additional 17 hours
  5. filtrationfiltered
  6. concentrationconcentrated to a volume of 100 ml
  7. customThe yellow solid that crystallized out
  8. filtrationwas collected by filtration
  9. washwashed
  10. customdried
  11. customto give the 6.05 g