HRID748107
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
A mixture of 2-mercapto-4-methylbenzoic acid (2.0 g, 12 mmol), 2-cyanopyridine (1.4 g, 13 mmol) and pyridine (8 ml) was refluxed for 14 hrs as described in Example 9. After cooling, the precipitated crystals were collected by filtration, subjected to a silica gel column chromatography, eluted with ethyl acetate-methanol (5:1, v/v) and recrystallized from hexane-tetrahydrofuran to give the titled compound (1.4 g, 48%).
WORKUP
后处理
- temperaturewas refluxed for 14 hrs
- temperatureAfter cooling
- filtrationthe precipitated crystals were collected by filtration
- washeluted with ethyl acetate-methanol (5:1
- customv/v) and recrystallized from hexane-tetrahydrofuran