Hydrochloric Acid → 13437-79-1

Temperature

0 °C

At room temperature 122 g of (R)-1-phenylethylamine (1.0 mol) was dissolved in 30 mL of isopropanol. The solution was stirred and cooled to 0° C. Then, a previously prepared solution of 100 mL of 37% hydrochloric acid (118 g, 1.2 mol) in 320 mL of isopropanol was added during 1 h. The solution was stirred at 0° C. for an additional 40 min, and then it was concentrated on a rotary evaporator (16 mbar, bath 45° C.) to a volume of 300 mL. The translucent gel which had formed was transferred into a 1.5 l flask, then, under stirring, 250 mL of tert-butyl-methyl-ether was slowly added. Crystals started to form and the suspension was stirred at 0° C. for 3 h. The product was collected by filtration, washed with 100 mL of tert-butyl-methyl-ether and dried at 30° C./16 mbar for 4 hours to give 133 g (84%) of 1-phenylethylamine hydrochloride.

1. stirringThe solution was stirred at 0° C. for an additional 40 min
2. concentrationit was concentrated on a rotary evaporator (16 mbar, bath 45° C.) to a volume of 300 mL
3. customThe translucent gel which had formed
4. customwas transferred into a 1.5 l flask
5. stirringunder stirring
6. customto form
7. stirringthe suspension was stirred at 0° C. for 3 h
8. filtrationThe product was collected by filtration
9. washwashed with 100 mL of tert-butyl-methyl-ether
10. customdried at 30° C./16 mbar for 4 hours

ORD record

ord-19070ecb7cfd4fb9b6e6600c13764e5f

Source dataset

uspto-grants-2001_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06274735B1