반응 #1687622

ord-60edf243ccb0493086a32b0c8e78a6a2

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타until acidic reaction
  2. 2
    여과The precipitate was filtered off
  3. 3
    기타dried
  4. 4
    workup.DISSOLUTIONdissolved in methanol (25 ml)
  5. 5
    workup.ADDITION5% palladium on charcoal (0.6 g) was added
  6. 6
    여과The catalyst was filtered off
  7. 7
    기타the filtrate was evaporated to dryness
  8. 8
    기타Crystallization from ethanol

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: USRE036374uspto-grants-1999_11