Hydrochloric Acid → 2-(2,3-Dimethylphenoxy)-2-methylpropanoic acid

Temperatur

50 °C

Sodium hydroxide (82.0 g, 2.05 mol) was added to a solution of methyl ethyl ketone (400 mL) containing 2,3-dimethylphenol (50.0 g, 410 mmol), and the mixture was stirred at 50° C. for 1 hour. After that, a solution of methyl ethyl ketone (200 mL) containing 2-bromo-2-methylpropionic acid (103 g, 615 mmol) was added thereto, and the mixture was stirred at 50° C. for 4 hours. After cooled to room temperature, the reaction solution was distributed by adding water and diethyl ether. 6N hydrochloric acid was added to the aqueous layer to be acidic, and then extraction was performed using ethyl acetate. The extract was washed with saturated saline, and then dried using anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the obtained residue was purified by silica gel chromatography (hexane-ethyl acetate 95:5 to 50/50) to give 38.3 g of the title compound (yield: 45%).

1. additionwas added
2. stirringthe mixture was stirred at 50° C. for 4 hours
3. temperatureAfter cooled to room temperature
4. extractionextraction
5. washThe extract was washed with saturated saline
6. customdried
7. customThe solvent was removed under reduced pressure
8. customthe obtained residue was purified by silica gel chromatography (hexane-ethyl acetate 95:5 to 50/50)

ORD-Eintrag

ord-bcdd452f0c374162b91c681230517bdd

Quelldatensatz

uspto-grants-2015_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08957069B2