反应详情

An 800 L still is charged with 53.9 kg (306 mol) of 3-benzoylacrylic acid. The 800 n still is charged with 41 kg (315 mol) of ethyl acetoacetate. The still is charged with 150 L of water. The agitator is started on the still. The still is charged with 56 kg (1475 mol) of 50% sodium hydroxide, followed by 20 L of water. The resulting solution is agitated, and the temperature of the contents is maintained at 45°-50° C. for 16 to 18 hours after the addition of the sodium hydroxide. The solution in the still is then refluxed for 20 to 24 hours (~100° C.). An 800 L reactor is charged with 140 L of water and 90.6 kg (1100 mol) of concentrated hydrochloric acid followed by 20 L of water, and the agitator is started. The reaction mixture in the still is cooled to 25°-40° C. The still is vented through the condenser to an atmospheric scrubber. The cooled solution in the still (25°-40° C.) is added to the diluted hydrochloric acid solution in the reactor at a rate of about 2-4 L/minute. The still is charged with 100 L of water, and this is transferred to the reactor. The resulting slurry in the reactor is agitated at 25°-40° C. for about 2 to 4 hours. The solid product in the reactor is filtered onto a centrifuge. The reactor is charged with 100 L water, and the water is directed to the cake on the centrifuge. The mother liquors and washes are discarded. The still is charged with 100 L water, the water is directed over the filter-cake, and the filtrate is discarded. The product wet cake from the centrifuge is returned to the still followed by 400 L of water, and the slurry is agitated for 2 to 4 hours. The solid product is filtered onto a centrifuge. The still and filter-cake are washed with 200 L of water. The filtrates are discarded. The water wet 5-oxo-3-phenyl-3-cyclohexenecarboxylic acid is transferred to a vacuum tray dryer and dried at 80°±5° C. for at least 24 hours using the best available vacuum to yield 62.5 kg of an off-white to pale yellow solid; mp 140°-160° C. (average of 2 determinations). The dry product is stored in plastic lined drums.

1. temperaturethe temperature of the contents is maintained at 45°-50° C. for 16 to 18 hours
2. temperatureThe solution in the still is then refluxed for 20 to 24 hours (~100° C.)
3. temperatureThe reaction mixture in the still is cooled to 25°-40° C
4. stirringThe resulting slurry in the reactor is agitated at 25°-40° C. for about 2 to 4 hours
5. filtrationThe solid product in the reactor is filtered onto a centrifuge
6. additionThe reactor is charged with 100 L water
7. additionThe still is charged with 100 L water
8. stirringthe slurry is agitated for 2 to 4 hours
9. filtrationThe solid product is filtered onto a centrifuge
10. filtrationThe still and filter-cake
11. washare washed with 200 L of water
12. customdried at 80°±5° C. for at least 24 hours
13. customto yield 62.5 kg of an off-white to pale yellow solid