Реакция #1687621
ord-ba9897736c6140dfa8ba13c48929a599
Уравнение реакции
Реагенты
Нет
Растворители
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1ФильтрацияThe mixture was filtered
- 2Другоеthe filtrate was evaporated
- 3workup.DISSOLUTIONThe residue was dissolved in dichloromethane (100 ml)
- 4Промывкаthe solution was washed three with water (100 ml)
- 5СушкаThe organic phase wan dried over magnesium sulphate
- 6Другоеevaporated
Методика
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.