Sodium Hydroxide → HCID 13671866, Verbindung

A mixture of (1RS,2SR)-2-amino-5-methyl-1-phenylhexan-1-ol (1.04 g, 5 mmol), 3-piperidinopropyl tosylate hydrochloride (2.00 g, 6 mmol) and sodium bicarbonate (1.05 g, 12.5 mmol) in ethanol (10 ml) was refluxed for 1 hour. After cooling, to the reaction mixture were added ether (100 ml), water (50 ml) and 2N-NaOH (5 ml) and the resulting mixture was well shaken. The ethereal layer was separated and washed three times with water, then once with brine, followed by drying and subsequent concentration under reduced pressure. The residue was dissolved in ethanol and to the solution was added 6N-HCl in EtOH (1.5 ml). Precipitated crystals were collected by filtration and then recrystallized from ethanol to obtain 0.73 g of the title compound as white crystals (yield: 36%).

1. temperaturewas refluxed for 1 hour
2. temperatureAfter cooling, to the reaction mixture
3. customThe ethereal layer was separated
4. washwashed three times with water
5. customby drying
6. concentrationsubsequent concentration under reduced pressure
7. dissolutionThe residue was dissolved in ethanol and to the solution
8. additionwas added 6N-HCl in EtOH (1.5 ml)
9. customPrecipitated crystals
10. filtrationwere collected by filtration
11. customrecrystallized from ethanol

ORD-Eintrag

ord-985c44c167284781af9b5eb92d5754d8

Quelldatensatz

uspto-grants-1993_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05250546