Реакция #1687621

ord-ba9897736c6140dfa8ba13c48929a599

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ФильтрацияThe mixture was filtered
  2. 2
    Другоеthe filtrate was evaporated
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in dichloromethane (100 ml)
  4. 4
    Промывкаthe solution was washed three with water (100 ml)
  5. 5
    СушкаThe organic phase wan dried over magnesium sulphate
  6. 6
    Другоеevaporated

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: USRE036374uspto-grants-1999_11