Hydrochloric Acid → 2-(3,5-Dimethyl-phenoxy)-1-methyl-ethylamine

Temperatur

130 °C

A 100 ml autoclave was charged with 1.96 g (9.8 mmol) of 1-(3,5-dimethylphenoxy)-2-chloropropane, 10 ml of ethanol and 0.2 g of sodium iodide, and then 40 ml of a 28% ammonia aqueous solution was added. The mixture was continuously stirred at 130° C. for 8 hours to complete the reaction. After allowed to cool, the reaction mixture was transferred into a 500 ml beaker with 50 ml of water and 20 ml of diethyl ether. A 20% hydrochloric acid aqueous solution was added to the reaction mixture until it became acidic, and the mixture was washed with 20 ml of diethyl ether three times. While the water layer was cooled, a 20% sodium hydroxide aqueous solution was added to make it alkaline, and the water layer was subjected to extraction with 50 ml of diethyl ether three times, and dried over 10 g of anhydrous sodium sulfate. Then, the solvent was distilled off under reduced pressure to give 1.48 g of 1-(3,5-dimethylphenoxy)-2-aminopropane (yield 83.7%).

1. customthe reaction
2. temperatureto cool
3. washthe mixture was washed with 20 ml of diethyl ether three times
4. temperatureWhile the water layer was cooled
5. additiona 20% sodium hydroxide aqueous solution was added
6. extractionthe water layer was subjected to extraction with 50 ml of diethyl ether three times
7. dry with materialdried over 10 g of anhydrous sodium sulfate
8. distillationThen, the solvent was distilled off under reduced pressure

ORD-Eintrag

ord-36a4dc3bc9f2489da306b91df0987b8e

Quelldatensatz

uspto-grants-1994_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05286905