반응 #1687621

반응 방정식

5-(3-pyridyl)-tetrazole

sodium hydroxide

methyl iodide

→

12

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

용매

ethanol

반응 조건

후처리

1. 1
   여과The mixture was filtered
2. 2
   기타the filtrate was evaporated
3. 3
   workup.DISSOLUTIONThe residue was dissolved in dichloromethane (100 ml)
4. 4
   세척the solution was washed three with water (100 ml)
5. 5
   건조The organic phase wan dried over magnesium sulphate
6. 6
   기타evaporated

실험 절차

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.

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