反応 #1687622

ord-60edf243ccb0493086a32b0c8e78a6a2

反応方程式

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

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他until acidic reaction
  2. 2
    ろ過The precipitate was filtered off
  3. 3
    その他dried
  4. 4
    workup.DISSOLUTIONdissolved in methanol (25 ml)
  5. 5
    workup.ADDITION5% palladium on charcoal (0.6 g) was added
  6. 6
    ろ過The catalyst was filtered off
  7. 7
    その他the filtrate was evaporated to dryness
  8. 8
    その他Crystallization from ethanol

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: USRE036374uspto-grants-1999_11