反应 #955908
ord-4b8a6dcbd4cc48d1b7d8f08cfcc08915
反应方程式
5-(2-methoxy-4-methylphenyl)-2H-1,2,4-triazole-3(4H)-thione
2-(bromomethyl)pyridine hydrobromide
→
desired product
收率 72.0%
2-((5-(2-methoxy-4-methylphenyl)-1H-1,2,4-triazol-3-ylthio)methyl)pyridine
收率 72.0%
试剂
无
反应条件
温度
60°CELSIUS
详细条件
See reaction.notes.procedure_details.
后处理
- 1洗涤washed with water, brine
- 2干燥dried over MgSO4
- 3过滤filtered
- 4其他evaporated
- 5其他to produce an oil
- 6其他The oil was purified on a preparative TLC plate
实验过程
To a solution of 5-(2-methoxy-4-methylphenyl)-2H-1,2,4-triazole-3(4H)-thione (Example 1a) (110 mg, 0.5 mmol) in 2 ml of EtOH was added 2-(bromomethyl)pyridine hydrobromide (152 mg, 0.6 mmol). The suspension was heated at 60° C. for 22 h. The reaction was diluted with EtOAc and washed with water, brine, dried over MgSO4 filtered and evaporated to produce an oil. The oil was purified on a preparative TLC plate to produce the desired product (72%). 1H NMR (500 MHz, CDCl3): δ 2.40 (s, 3H), 3.99 (s, 3H), 4.55 (s, 2H), 6.84 (s, 1H), 6.92-6.93 (d, 1H), 7.16-7.19 (dd, 1H), 7.53-7.55 (d, 1H), 7.62-7.65 (m, 1H), 8.15-8.17 (d, 1H), 8.56-8.57 (d, 1H). MS (M+H, 313).