Ammonia → HCID 20346679, compound

HRID 1701477Notes

Reaction equation

HRID 1701477 reaction equation
[CH3:1][C:2]1[CH2:6][CH:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[NH:4][N:3]=1.N>[Ni].CO>[CH3:1][CH:2]([NH2:3])[CH2:6][CH:5]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1)[NH2:4]

Participants

5

Reactant 2

HCID 222AmmoniaHCID 101301011H-Pyrazole, 4,5-dihydro-3-methyl-5-phenyl-

Product 1

HCID 20346679HCID 20346679, compound

Reagents, catalysts & solvents 2

HCID 935NickelCatalystHCID 887MethanolSolvent

Procedure

160 g (1 mol) of 3-methyl-5-phenyl-2-pyrazoline (according to S. G. Beech et al, J. Chem. Soc. (1952) 4,686-90) are hydrogenated with 20 g of freshly prepared Raney nickel in 400 ml of methanol saturated with NH3 for 6 hours at 80° C./100 atmospheres. The catalyst is separated off, the solvent is removed in a rotary evaporator and the product is distilled under a high vacuum. Fractionation of the distillate in a 25 cm Vigreux column gives 151 g=92% of theory of a colourless oil with a boiling point under 0.03 mm of 90°-91° C. C10H16N2 . (164.24)

Workup

  1. customThe catalyst is separated off
  2. customthe solvent is removed in a rotary evaporator
  3. distillationthe product is distilled under a high vacuum
  4. customFractionation of the distillate in a 25 cm Vigreux column gives 151 g=92% of theory of a colourless oil with a boiling point under 0.03 mm of 90°-91° C

Sources & evidence

ORD record
ord-7614208fe75848b0ad2157b13d9ac585
Source dataset
uspto-grants-1980_03
Patent number
US04193905

Reaction notes

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