[NH2:1][C:2]([CH3:9])([CH2:5][CH:6]([CH3:8])[CH3:7])[C:3]#[N:4].Cl[O-].[Na+].S([O-])([O-])(=O)=S.[Na+].[Na+].Cl.N([O-])=O.[Na+]>O.CO>[N:1]([C:2]([CH3:9])([CH2:5][CH:6]([CH3:8])[CH3:7])[C:3]#[N:4])=[N:1][C:2]([CH3:9])([CH2:5][CH:6]([CH3:8])[CH3:7])[C:3]#[N:4]To a solution of 63.2 parts of 2-amino-2,4-dimethylpentanonitrile in 592 parts of methanol are added over a 20 minute period at -10°C. with agitation 377 parts of a 15% aqueous sodium hypochlorite solution. The reaction was then allowed to warm to 10°C. and held for 10 minutes. At this point methanol constitutes 74 volume percent of the aqueous solvent. The resulting reaction product was diluted with 500 parts of water and titrated with standard sodium thiosulfate as described in Example 1. About 0.015 equivalent of oxidizing agent was present. The resulting slurry was then acidified to a pH of 1.0 with 15% hydrochloric acid and 0.52 gram of sodium nitrite (0.015 equivalent) were stirred into the mixture. The precipitated 2,2'-azobis (2,4-dimethylvaleronitrile) was isolated by filtration and found to be non-oily, white and dry with a purity of 98%.
Wird geladen…
