Preparation of perchloro-2,5-diaza-1,5-hexadiene

Details Preparation of perchloro-2,5-diaza-1,5-hexadiene Preparation of perchloro-2,5-diaza-1,5-hexadiene

1978-12-29

1980-09-30

Trousof, Natalie

Chemistry of carbon compounds

Miscellaneous organic carbon compounds

C-metal

260566R, C07C11900

Patent

active

042255104

ABSTRACT:
In the preparation of perchloro-2,5-diaza-1,5-hexadiene by chlorination of N,N-dimethylaminoacetonitrile, the improvement which comprises in a first stage (a) chlorinating N,N-dimethylaminoacetonitrile or its hydrochloride at about 70.degree. to 80.degree. C. in a solvent, removing the solvent by distillation under chlorinating conditions until a bottom temperature of about 120.degree. to 160.degree. is reached, and after-treating the residual reaction at this temperature with chlorine, and in a second stage (b) chlorinating the resulting reaction mixture at a temperature from about 150.degree. to 220.degree. C. Advantageously the solvent in stage (a) is phosphorus oxychloride, the weight ratio of nitrile to solvent is about 1:3, the after-chlorination in stage (a) is carried out at a temperature from about 120.degree. to 140.degree. C., and stage (b) is carried out at a temperature from about 180.degree. to 210.degree. C. in a multi-stage bubble column cascade reactor operated with gas and liquid in counter-current.

REFERENCES:
patent: 3206516 (1965-09-01), Ziegenbein et al.
patent: 3251760 (1966-05-01), Holtschmidt et al.
patent: 3267144 (1966-08-01), Ottmann et al.
patent: 3301893 (1967-01-01), Degener et al.
Beck, von Gunther et al. Angew. Chem., vol. 86, p. 134 (1974).

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