反应详情

A clean dry reactor of 50 gallon capacity (227 liters) was charged with glacial acetic acid (92.0 kg.). With agitation benzoin hemisuccinate (25.3 kg.) prepared as described under part A and ammonium acetate (31 kg.) were added. The reaction mixture was heated to 90°-95° C. and stirred at this temperature range for 11/2 hours. Water (44.0 kg.) was carefully added to the reaction mixture and the mixture was reheated to 90°-95° C. The mixture was then transferred to another reactor of 50 gallon capacity (227 litres) through a pre-heated pressure filter. The first reactor and the filter were washed through with a mixture of glacial acetic acid (13.3 kg.) and water (6.2 kg.). The mixture in the reactor was then cooled to 10°-15° C. with agitation and the product was filtered on a ceramic filter. The product on the ceramic filter was then washed with a mixture prepared by adding glacial acetic acid (25.5 kg.) with agitation to water (12.5 kg.). The product on the filter was sucked well dry and then washed with demineralised water (10 kg.) and sucked well dry. The product was dried in a Mitchell oven at 80° C. for 16-18 hours. The yield of crude β-(4,5-diphenyloxazol-2-yl)propionic acid was 17.5 kg. (67% overall yield for parts A and B).

1. additionwere added
2. temperatureThe reaction mixture was heated to 90°-95° C.
3. customwas reheated to 90°-95° C
4. customThe mixture was then transferred to another reactor of 50 gallon capacity (227 litres) through a pre-heated pressure
5. filtrationfilter
6. washThe first reactor and the filter were washed through with a mixture of glacial acetic acid (13.3 kg.) and water (6.2 kg.)
7. temperatureThe mixture in the reactor was then cooled to 10°-15° C. with agitation
8. filtrationthe product was filtered on a ceramic filter
9. filtrationThe product on the ceramic filter
10. washwas then washed with a mixture
11. customprepared
12. customThe product on the filter was sucked well dry
13. washwashed with demineralised water (10 kg.)
14. customsucked well dry
15. customThe product was dried in a Mitchell oven at 80° C. for 16-18 hours
16. custom(67% overall yield for parts A and B)