反应 #1687622

ord-60edf243ccb0493086a32b0c8e78a6a2

反应方程式

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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

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