Hydrochloric Acid → HCID 4135652, compound

Pentyl 3,4-dipentyloxybenzoate (911 mg, 2.50 mmol) was dissolved in methanol (15.0 ml). To this solution was added a 1N aqueous potassium hydroxide solution (7.5 ml, 7.5 mmol, 3 eq), and the mixture was stirred with reflux for 5 hours. A 3N aqueous hydrochloric acid solution was added to this reaction mixture to make the same acidic (pH <2). The mixture was extracted with chloroform (20 ml×3). The organic layer was washed with saturated brine (20 ml). The organic layer was d ried over anhydrous magnesium sulfate, and the drying agent was filtered off. The filtrate was concentrated under reduced pressure to give a colorless solid. This was recrystallized from ethyl acetate-hexane to give 3,4-dipentyloxybenzoic acid (512 mg, 70%) as colorless crystals.

1. temperaturewith reflux for 5 hours
2. extractionThe mixture was extracted with chloroform (20 ml×3)
3. washThe organic layer was washed with saturated brine (20 ml)
4. filtrationthe drying agent was filtered off
5. concentrationThe filtrate was concentrated under reduced pressure
6. customto give a colorless solid
7. customThis was recrystallized from ethyl acetate-hexane

ORD record

ord-05ba9f8f246a41dfbf437ae0b213221f

Source dataset

uspto-grants-2000_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06017919