DE890947C - Process for the preparation of butanediol- (1, 4) -one- (2) - Google Patents

Description

Process for the preparation of butanediol- (1, 4) -one- (2) subject of the Patent 750 057 is a method of making. Butdndiol- (i, 4) -o-n- (2), in which in the liquid phase butyne - (2) -diol- (i, 4) and wasiser with acidic oils are verb @ i @ ndunngen mixed well, then the reaction mixture neutralized and, if necessary, removed the butanediol- (i, 4) -one- (2) formed by distilling off the neutralized solution of the water isolated under reduced pressure.

It has now been found that one; also butanediol- (i, 4) -one (2) obtained if the starting material used instead of butynediol is oxymethyl vinyl ketone [buten- (i) -one (3) -01- (4) 1 used. The Oxymethylvinylk.eton is with the. Butynediol isomer and forms; when treating butind6.oi1 with acidic compounds of mercury, Silver and copper.

The reaction proceeds so easily that an aqueous solution is sufficient of oxymethylvinyllc.etone with an acidic mercury compound, z. B. mercuric sulfate or acetate, mix well. The implementation is already taking place at ordinary temperature, but it is advisable to help accelerate them elevated temperature, e.g. B. at 40 to 70 °, and in the presence of a small amount free acid to work.

Since the butanediolone has a very strong tendency to self-condense, it works Here too, in order to avoid this further condensation, it is best to use a dilute solution Solution and within. of the specified Temperature range. Further it is advisable to test the effect of this catalyst by neutralizing the solution to be interrupted as soon as the accumulation of water has ended, which can easily be seen by observing the bromine count the implementation solution can determine.

You also have to work on it. on the easy condensation ability of the butanediolone. For many purposes one therefore uses the one where Reaction obtained aqueous solution after neutralizing the free acid immediately, optionally after removal of the catalyst. But you can also use the butanediolone after neutralizing the reaction solution while distilling off the water isolate under reduced pressure. But already with this distillation: des Water, in particular, however. by. Distillation of the butanediolone under reduced Pressure, the yield is greatly reduced, since this is already the further condensation entry.

The ones below. The parts given in the example are parts by weight.

Example 500 parts of an approximately 100% aqueous oxymethyl vinyl ketone solution, whose carbonyl number is 63 and bromine number 16.1, 3 parts of mercury sulfate are added and parts of concentrated sulfuric acid. Maintain the temperature while stirring well of the reaction mixture for 8 hours at 50 to 55 ° and monitored by removal smaller samples. the drop in the bromine number. After 4 and 6 hours. Implementation time will be three more parts each of mercuric sulfate added to the reaction mixture. To 8 hours. the bromine number has practically the. Reached zero while the carbonyl number remains unchanged.

The solution is neutralized by adding potassium carbonate. she contains butaned @ iol- (1,4) -on.- (2) in 65% yield, as can be seen from the amount of the butanetriol (Z, 2, 4) obtained therefrom in the catalytic hydrogenation.

Claims (1)

PATENT CLAIM: Further training of the manufacturing process of butanediol- (1, 4) -one- (2) according to patent 750057, characterized in that one instead of. Butyni- (2) -diol- (z, 4) used as the starting material oxymethyl vinyl ketone.