HRID1940907
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
8-Amino-2-benzylthio[1,2,4]triazolo[1,5-a]pyridine (25.6 g, 0.1 mol), N-bromosuccinimide (17.8 g, 0.1 mol) and 2 L of dichloromethane were combined with stirring for an hour. The solution was washed with dilute aqueous sodium bisulfite and then with water and the volatiles were removed by evaporation under reduced pressure. The residue obtained was chromatographed on silica gel eluting with 25 percent ethyl acetate in hexane. The product fractions were concentrated by evaporation under reduced pressure and the solid residue obtained was extracted with ether and dried to obtain 17.5 g (52 percent of theory) of the title compound as a light tan powder melting at 125°-126° C.
WORKUP
后处理
- washThe solution was washed with dilute aqueous sodium bisulfite
- customwith water and the volatiles were removed by evaporation under reduced pressure
- customThe residue obtained
- customwas chromatographed on silica gel eluting with 25 percent ethyl acetate in hexane
- concentrationThe product fractions were concentrated by evaporation under reduced pressure
- customthe solid residue obtained
- extractionwas extracted with ether
- customdried