Potassium Cyanide → HCID 19752109, Verbindung

Temperatur

20 °C

Bicyclo[3.2.1]octan-2-one (30 g) is dissolved in ethanol (300 cc) and a solution of potassium cyanide (18.2 g) and ammonium chloride (13.9 g) in water (300 cc) is added. After stirring for 6 days at 20° C., the ethanol is concentrated under reduced pressure (5.2 kPa) and the aqueous phase is extracted with diethyl ether (5×200 cc). The ethereal phase is washed with water (2×50 cc), dried over sodium sulphate and concentrated under reduced pressure (5.2 kPa) to a volume of 400 cc. Hydrogen chloride gas is then bubbled through the solution until it is saturated. The precipitate formed is drained, washed with diethyl ether (3×25 cc) and dried under reduced pressure (2.5 kPa). 2-Amino-2-cyano-bicyclo[3.2.1]octane hydrochloride (13.25 g) is thus obtained, as a mixture of the exo and endo racemates in a ratio of (8/1), in the form of fine white crystals which melt with decomposition at 202°-5° C.

1. concentrationthe ethanol is concentrated under reduced pressure (5.2 kPa)
2. extractionthe aqueous phase is extracted with diethyl ether (5×200 cc)
3. washThe ethereal phase is washed with water (2×50 cc)
4. dry with materialdried over sodium sulphate
5. concentrationconcentrated under reduced pressure (5.2 kPa) to a volume of 400 cc
6. customHydrogen chloride gas is then bubbled through the solution until it
7. customThe precipitate formed
8. washwashed with diethyl ether (3×25 cc)
9. customdried under reduced pressure (2.5 kPa)

ORD-Eintrag

ord-24faf0c554904b76aa2c71e134079af3

Quelldatensatz

uspto-grants-1993_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05225207