تفاعل #1687621

ord-ba9897736c6140dfa8ba13c48929a599

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحThe mixture was filtered
  2. 2
    أخرىthe filtrate was evaporated
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in dichloromethane (100 ml)
  4. 4
    غسيلthe solution was washed three with water (100 ml)
  5. 5
    تجفيفThe organic phase wan dried over magnesium sulphate
  6. 6
    أخرىevaporated

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: USRE036374uspto-grants-1999_11