تفاعل #1687622

ord-60edf243ccb0493086a32b0c8e78a6a2

معادلة التفاعل

Cn1nnc(-c2cccnc2)n1
12
Cn1nnc(-c2cccnc2)n1
2-Methyl-5-(3-pyridyl)-2H-tetrazole
Cl
hydrogen chloride
Cl.Cn1nnc(C2CCCNC2)n1
title product
المردود 26.0%
Cl.Cn1nnc(C2CCCNC2)n1
2-Methyl-(3-piperidyl)-2H-tetrazole, hydrochloride
المردود 26.0%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىuntil acidic reaction
  2. 2
    ترشيحThe precipitate was filtered off
  3. 3
    أخرىdried
  4. 4
    workup.DISSOLUTIONdissolved in methanol (25 ml)
  5. 5
    workup.ADDITION5% palladium on charcoal (0.6 g) was added
  6. 6
    ترشيحThe catalyst was filtered off
  7. 7
    أخرىthe filtrate was evaporated to dryness
  8. 8
    أخرىCrystallization from ethanol

الإجراء التجريبي

To a solution of 12 (1.93 g, 0.012 mol) in acetone (50 ml) was added hydrogen chloride in ether until acidic reaction. The precipitate was filtered off, dried, and dissolved in methanol (25 ml). 5% palladium on charcoal (0.6 g) was added, and the mixture was shaked overnight under 3 atm. of hydrogen pressure. The catalyst was filtered off and the filtrate was evaporated to dryness. Crystallization from ethanol yielded 0.63 g (0.0031 mol, 26%) of title product M.P. 168°-172° C. Anal. (C7H14ClN5) C, H, N.

المصدر

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