Ethyl valerate → Acetophenone

A total of 9 Fernbach flasks, each containing 500 ml. broth, were sterilized for 30 minutes at 121° C. After cooling to room temperature, 5.0 ml. of sterile 50% dextrose solution and 5.0 ml of the 24 hour grown inoculum were added to each flask. The flasks were incubated at 30° C. at 100 rpm for 24 hours. Sterile 10% sodium cinnamate, pH 7.0, was added to each flask as follows, 5 g/l at 24 hours, 9 g/l at 48 hours, and 6 g/l at 72 hours. Samples of broth were analyzed periodically, by GC using ethyl pentanoate as an internal standard. After 44 hours of incubation, all the flasks were combined and product was extracted 3 times with ethyl acetate (approximately 1/2 volume each time). The combined extracts were washed 2 times with 100 ml. saturated NaHCO3 each time, followed by 2 times 100 ml saturated NaCl washes. The solvent was removed under vacuum and the crude extract was fractionally distilled to recover product. A yield of 2.7 g/L having a purity of 99.4% was obtained.

1. additionwere added to each flask
2. waitThe flasks were incubated at 30° C. at 100 rpm for 24 hours
3. wait5 g/l at 24 hours
4. wait9 g/l at 48 hours
5. wait6 g/l at 72 hours
6. waitAfter 44 hours of incubation
7. extractionproduct was extracted 3 times with ethyl acetate (approximately 1/2 volume each time)
8. washThe combined extracts were washed 2 times with 100 ml
9. customThe solvent was removed under vacuum
10. extractionthe crude extract
11. distillationwas fractionally distilled
12. customto recover product
13. customwas obtained

ORD record

ord-60e5e93b25dc4032ae5382e1114e995f

Source dataset

uspto-grants-2000_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06165517