تفاعل #9797

معادلة التفاعل

4-hydroxybenzophenone

N-methylpyrrolidone

→

4-vinyloxybenzophenone

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas charged
2. 2
   أخرىflushed with nitrogen
3. 3
   أخرىDuring the reaction, further acetylene
4. 4
   أخرىthat consumed by reaction
5. 5
   درجة الحرارةso as to maintain a constant pressure of 20 bar
6. 6
   درجة الحرارةAfter a reaction time of 12 hours the batch was cooled to 20–25° C. (room temperature)
7. 7
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure at a bridge temperature of from 70 to 80° C. with a pressure of 1 mbar (absolute)
8. 8
   workup.ADDITION310 g of Pluriol® E 600 (polyethylene glycol, trademark of BASF AG) were then added
9. 9
   workup.DISTILLATIONthe product was purified by a Sambay distillation at 1.2 mbar (absolute)
10. 10
    أخرىa bridge temperature of 163° C

الإجراء التجريبي

A mixture of 650 g of 4-hydroxybenzophenone (98% by weight, Avocado, Research Chemicals Ltd.), 750 ml of N-methylpyrrolidone (>99% by weight, BASF AG) and 60 g of zinc naphthenate (Nusa; zinc salts of naphthenic acids, zinc content 12% by weight) was charged with stirring to a 2.5 l autoclave and flushed with nitrogen. After it had been heated to 190° C., injection was carried out first with nitrogen to 2 bar and then with acetylene to 20 bar. During the reaction, further acetylene was supplied to replace that consumed by reaction, so as to maintain a constant pressure of 20 bar. After a reaction time of 12 hours the batch was cooled to 20–25° C. (room temperature) and let down to atmospheric pressure. The solvent was distilled off under reduced pressure at a bridge temperature of from 70 to 80° C. with a pressure of 1 mbar (absolute). 310 g of Pluriol® E 600 (polyethylene glycol, trademark of BASF AG) were then added and the product was purified by a Sambay distillation at 1.2 mbar (absolute) and a bridge temperature of 163° C. This gave a total of 522 g of 4-vinyloxybenzophenone having a purity of from 96 to 99% by weight and a melting point of 58° C.

المصدر