HRID2051774
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
1.0 g of 1H-Naphth[2,3-d]imidazole-2-thiol and 0.8 g of 2-chloromethylimidazole-hydrochloride were heated for 11/2 hours at 90° in 20 ml of dimethylformamide. The precipitate formed was filtered off, washed with a small amount of acetonitrile, and dissolved in 2 N sodium bicarbonate solution. The aqueous phase was extracted three times with 30 ml of ethyl acetate. The organic phases were washed with saturated sodium chloride solution, dried over magnesium sulphate, and then concentrated by evaporation. The residue was recrystallised from 150 ml of acetonitrile. 150 mg of 2-[(Imidazole-2-ylmethyl)thio]-1H-naphth[2,3-d]imidazole having a melting point of 172° was obtained.
WORKUP
后处理
- customThe precipitate formed
- filtrationwas filtered off
- washwashed with a small amount of acetonitrile
- dissolutiondissolved in 2 N sodium bicarbonate solution
- extractionThe aqueous phase was extracted three times with 30 ml of ethyl acetate
- washThe organic phases were washed with saturated sodium chloride solution
- dry with materialdried over magnesium sulphate
- concentrationconcentrated by evaporation
- customThe residue was recrystallised from 150 ml of acetonitrile