反应 #1687621

反应方程式

5-(3-pyridyl)-tetrazole

sodium hydroxide

methyl iodide

→

12

2-Methyl-5-(3-pyridyl)-2H-tetrazole

溶剂

ethanol

反应条件

后处理

1. 1
   过滤The mixture was filtered
2. 2
   其他the filtrate was evaporated
3. 3
   workup.DISSOLUTIONThe residue was dissolved in dichloromethane (100 ml)
4. 4
   洗涤the solution was washed three with water (100 ml)
5. 5
   干燥The organic phase wan dried over magnesium sulphate
6. 6
   其他evaporated

实验过程

5-(3-pyridyl)-tetrazole (11) (J. M. McManus and R. M. Herbst, J. Am. Chem. Soc., 24 (1959) 1462-64) (10 g, 0.068 mol), sodium hydroxide (2.73 g, 0.068 mol), and methyl iodide (14.5 g, 0.1 mol) in ethanol (100 ml) was stirred at 40° C. overnight. The mixture was filtered and the filtrate was evaporated. The residue was dissolved in dichloromethane (100 ml), and the solution was washed three with water (100 ml). The organic phase wan dried over magnesium sulphate and evaporated yielding 3.21 g (0.020 mol 30%) of 12 with M.P. 108°-110° C. According to the 1H NMR spectrum the product contained less than 10% of the 1-isomer.

来源