HRID1702847
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationfiltered
- additionThe filtrate was added to 5.650 g
- temperatureat reflux under a nitrogen atmosphere for 6 hours
- stirringstirred an additional 17 hours
- filtrationfiltered
- concentrationconcentrated to a volume of 100 ml
- customThe yellow solid that crystallized out
- filtrationwas collected by filtration
- washwashed
- customdried
- customto give the 6.05 g