Piperidine → HCID 178420895, compound

HRID 1732147Notes

Reaction equation

HRID 1732147 reaction equation
Cl.Cl[CH2:3][C:4]1[N:8]=[CH:7][NH:6][N:5]=1.[NH:9]1[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1>>[N:9]1([CH2:3][C:4]2[N:8]=[CH:7][NH:6][N:5]=2)[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10]1

Participants

3

Reactant 2

HCID 8082PiperidineHCID 178478569HCID 178478569, compound

Product 1

HCID 178420895HCID 178420895, compound

Procedure

3-Chloromethyl-1,2,4-triazole hydrochloride (0.5 g.) was added to piperidine (10 ml.) and the mixture was heated at 100° for 16 hours, then evaporated to dryness. The residue was dissolved in water (10 ml.) and basified with sodium bicarbonate. The resulting solution was evaporated to dryness and the residue was extracted twice with ethanol (50 ml.). The combined extracts were evaporated to dryness and the residual gum was subjected to MPLC on K60 silica gel using methanol/chloroform, 3/97 v/v, as solvent to give 3-(piperidinomethyl)-1,2,4-triazole with NMR data as follows: solvent--CDCl3 : 8.05 ppm (singlet, 1H), 3.75 ppm (singlet, 2H), 2.5 ppm (multiplet, 4H) and 1.6 ppm (multiplet, 6H).

Workup

  1. temperaturethe mixture was heated at 100° for 16 hours
  2. customevaporated to dryness
  3. dissolutionThe residue was dissolved in water (10 ml.)
  4. customThe resulting solution was evaporated to dryness
  5. extractionthe residue was extracted twice with ethanol (50 ml.)
  6. customThe combined extracts were evaporated to dryness

Sources & evidence

ORD record
ord-31b09895d2a644498f07f57d873e0eba
Source dataset
uspto-grants-1986_11
Patent number
US04625036

Reaction notes

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