Ammonia → HCID 20346679, compound
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
Product 1
Reagents, catalysts & solvents 2
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
- customThe catalyst is separated off
- customthe solvent is removed in a rotary evaporator
- distillationthe product is distilled under a high vacuum
- 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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