Sulfuric Acid → HCID 19880030, compound

Then, 180 g of 85% KOH was dissolved in 180 ml of water, and 190 g of the above ethyl 5-methoxy-2-ethoxycarbonylcaprylate was dropped at 20°-30° C. in 60 min., followed by 30 min. of stirring and 2 hours of refluxing. After cooling, the mixture was held below 20° C., and a solution of 288 g of conc. sulfuric acid in 406 g of water was dropped in 90 min., followed by 30 min of stirring and 3 hours of refluxing at 90°-95° C. After being cooled to room temperature, the product was extracted with ether. The ether layer was washed with 5%-NaOH aqueous solution and added to the aqueous layer. The aqueous layer was acidified with 6N-hydrochloric acid and extracted with ether, followed by washing with saturated saline water, distilling-off of the ether and vacuum distillation to obtain 53 g of 5-methoxycaprylic acid in the form of a colorless clear liquid.

1. temperatureof refluxing
2. temperatureAfter cooling
3. customwas held below 20° C.
4. waitfollowed by 30 min
5. stirringof stirring and 3 hours
6. temperatureof refluxing at 90°-95° C
7. extractionthe product was extracted with ether
8. washThe ether layer was washed with 5%-NaOH aqueous solution
9. additionadded to the aqueous layer
10. extractionextracted with ether
11. washby washing with saturated saline water, distilling-off of the ether and vacuum distillation

ORD record

ord-261fc9e758fb412c8e7ca2a283d761da

Source dataset

uspto-grants-1992_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05143643