DE164755C - - Google Patents

Description

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GREAT

By the action of hypochlorite or hypobromite salts on urea or its Derivatives (which are formed by replacing the hydrogen atoms in the amide group) are obtained to hydrazine according to the following reaction:

^co \

, NH Na OCl = CO

₂ + Na Cl + NH ₂ · NH ₂

10

+ NaO Cl = CO ₂ + NaCl + NH ₂ - NHR.

In order to obtain a better yield of hydrazine and its derivatives, one must too great an excess of hypochlorite and hypobromite salts (more than the theoretical Amount thereof is) to avoid carrying out the reaction at a low temperature and, in order to prevent a Decomposition of the hydrazine, the action

ao continue in the presence of aldehydes or ketones, with the hydrazine in the corresponding Aldazine or Ketazine is transferred.

One takes z. B. 60 g urea and about 100 g sodium hydroxide, dissolves in a ge ^a wrestling amount of water, cools the solution to a temperature not above + 5 ⁰ C. and adds up to 2500 ecm of a solution of sodium hypochlorite, which previously Was cooled to this temperature and contains 30 g Na O Cl per liter. 150 to 200 g of benzaldehyde are added to this mixture, the mixture is mixed thoroughly and the excess aldehyde is then driven off by passing in steam for 10 to 15 minutes. Then new.

if you neutralize the above mixture, z. B. with sulfuric acid, the benzaldazine formed C ₁₄ H ₁₂ N ₂ (together with a small amount of benzal semicarbazide C ₈ H ₀ N ₈ O) filtered after cooling sufficiently and decomposed by heating with mineral acids into hydrazine salts and benzaldehyde.

For the preparation of the hydrazine it is not necessary to start from pure urea. Ordinary human or animal urine can also be used for this purpose. In the amount of urine used, the amount by weight of urea contained therein is determined, and a corresponding amount of sodium hydroxide is then dissolved in it. The solution is cooled and mixed with a solution of sodium hypochlorite and benzaldehyde. The bodies used here can be carried out in the same weight ratios and the entire procedure under the same conditions as described above for the use of pure urea as the starting material . '■ · ■■ ·. ■

In the representation of the derivatives of the hydra-

interest one uses the corresponding derivatives of urea; You can proceed as indicated above, but with the difference that the addition of the aldehydes or ketones is not necessary. So z. B. for the preparation of benzoylhydrazine (C- H _s JV ₂ O) 164 g of benzoylurea and 80 g of sodium hydroxide mixed with a small amount of water, it is then cooled to below + 5 ° C. and 2.5 1 of a cooled solution of Sodium hypochlorite, which contains 30 g of this salt per liter, is added. After the benzoylurea has dissolved, this solution is heated for some time to 70 to 80 ^° C. The benzoyl hydrazine (together with a small amount of dibenzoyl hydrazine) precipitates out of the solution.

Instead of sodium hypochlorite,

ao one calcium hypochlorite and other hypochlorites or hypobromite, as well as a derivative of iodine acid, e.g. B. Use iodosobenzene (C _n H ₁ JO) . In addition to benzaldehyde, room octaldehyde, acetaldehyde, anisaldehyde, glucose, acetone and other aldehydes and ketones are also suitable for the preparation of hydrazine and its derivatives.

Claims (1)

Patent claim: Process for the preparation of hydrazine and its acidyl, alkyl or aryl derivatives, characterized in that urea and its acidyl, Alkyl or aryl derivatives Hypochloritbezw. Hypobromite salt solutions in approximately molecular ratio at low temperature, expediently in the presence of aldehydes or ketones. BERLIN. PRINTED IN THE EMPIRE PRINTING.