HRID499512
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-Cyanopyridine (0.29 g, 2.8 mmol) and 4-bromothiosalicylic acid (0.8 g, 3.4 mmol) were dissolved in pyridine (6 ml), and the mixture was refluxed for 8 hrs. The solvent was evaporated, and the residue was subjected to silica gel column chromatography. The fractions eluted with chloroform-ethyl acetate (5:1, v/v) were collected, concentrated and recrystallized from hexane-chloroform to give the titled compound (0.33 g, 36%) as white crystals.
WORKUP
后处理
- temperaturethe mixture was refluxed for 8 hrs
- customThe solvent was evaporated
- washThe fractions eluted with chloroform-ethyl acetate (5:1
- customv/v) were collected
- concentrationconcentrated
- customrecrystallized from hexane-chloroform