DE84389C - - Google Patents

Description

IMPERIAL

PATENT OFFICE.

of their salts.

I. Replacing the diazo compound in Example I of Patent Specification No. 81202 of aniline by that of ß-naphtylamine so becomes the potassium salt of ß-naphtylnitrosamine obtain; the procedure can also be modified in such a way that the Introduces solution of the diazo compound into the heated liquor. The sodium salt is like at other nitrosamines of primary bases also here more difficultly soluble than the potassium salt and therefore particularly suitable for deposition.

Example:

10 parts by weight of an ioproc. Solutions of β-diazonaphthalene chloride are slowly introduced into a solution of 25 parts by weight of potassium hydrate in 5 parts by weight of water, heated to 120 ° C., with thorough stirring, whereby the nitrosamine potassium, which is very sparingly soluble in the concentrated potassium hydroxide solution, is deposited on the surface in the form of shiny gray grains. After entering the diazo solution, the temperature of the melt is so long maintained at 120 ⁰ C. and increased to 150 ⁰ C., until, with the aid of Naphtolprobe Diazonaphtalinkalium is no longer detectable. The precipitated ß-naphthylnitrosamine potassium is separated from the mother liquor while still hot and, after pressing, dissolved in water for further purification and precipitated as sodium salt in small pearlescent crystals.

II. In which Patent Supplement No. 81204 is describes a process for the preparation of nitrosamines of primary aromatic amido compounds, consisting in that the nitroso compounds of the acid derivatives of these amido compounds with alkalis. treated, up a sample, diluted with water and mixed with a solution of ß-naphtol sodium, there is no more dye formation.

It has been shown that the nitroso compounds of the acid derivatives of β-naphthylamine be converted into the nitrosamine of ß-naphtylamine by this process can.

Example:

50 parts by weight of a 2oproc. Aqueous paste of the nitroso compound of acet-β-naphthalide is stirred into 140 parts by weight of powdered potassium hydrate and processed with it until a uniform, thick paste is obtained. This is then heated to 120 to 130 ⁰ C., gives no more dye to a sample after dilution with water with ß-Naphtolnatriumlösung what long after about 1 5 minutes heating is the case. Naphtylnitrosaminkalium by suction - after the mass is cooled to 50 ⁰ C., which is β

(2nd edition, issued October 26th

and pressing separated from the potassium hydroxide solution. By dissolving in water and filtering can get the ß-naphtylnitrosamine potassium from a Separate small amounts of insoluble by-products and remove them from the solution by means of potassium hydrate as potash salt or by sodium hydrate or table salt in the form of the less soluble Separate the sodium salt. The formation of ß-naphthylnitrosamine potassium also takes place in Temperatures below 100 ° C, but much more slowly.

Claims (2)

Patent claims: i. The special embodiment of the claim ι of the main patent no. 78874 and claim 3 of the amendment to patent no. 81202 for the protected process Representation of salts of β-naphthylnitrosamine, consisting in the fact that the Diazo compound of ß-naphtylamine heated with solutions of alkaline solutions until one Sample of the mixture, diluted with water and mixed with an alkaline solution of ß-naphthol, no more dye forms. 2. The special embodiment of claim 1 of main patent no. 78874 and Supplementary Patent No. 81204 Process consisting in that the nitroso compounds of the acid derivatives of β-naphthylamine are mixed with solutions Treated by caustic alkalis until a sample, diluted with water, with ß-naphto-sodium mixed, shows no more dye formation.