Reaktion #96206

Reaktionsgleichung

1-(3,5-bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne

sulphuric acid

→

1-(3,5-bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne hydrogensulphate

Lösungsmittel

diethyl ether

diethyl ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationfiltered
2. 2
   WaschenThe solid residue was washed with anhydrous diethyl ether (2×20 ml)
3. 3
   Trocknendried over phosphorus pentoxide at a pressure of 0.01 mg Hg for 48 hours

Vorschrift

A stirred solution of 1-(3,5-bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne (0.98 g) in anhydrous diethyl ether (50 ml) was treated with a solution of sulphuric acid (e.g. 1.84) in anhydrous diethyl ether (0.25 molar solution; 10 ml). The mixture was allowed to stand for 30 minutes and then filtered. The solid residue was washed with anhydrous diethyl ether (2×20 ml) and dried over phosphorus pentoxide at a pressure of 0.01 mg Hg for 48 hours, to give 1-(3,5-bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne hydrogensulphate (1.15 g), m.p. 221°-222° C. in the form of a white powder which had the elementary analysis C: 49.1%; H: 5.02%; N: 2.76% (C20H25F6NO4S requires C: 49.07%; H: 5.15%; N: 2.86%).

Quelle