Reaktion #96204

Reaktionsgleichung

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

methanesulphonic acid

→

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

Ausbeute 95.4%

Lösungsmittel

diethyl ether

diethyl ether

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturcooled
2. 2
   SonstigeThe solid precipitate was removed by filtration
3. 3
   Waschenwashed with cold anhydrous diethyl ether
4. 4
   Sonstigedried at 0.05 mm Hg for 2 hours

Vorschrift

A solution of 1-(3,5-bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne (9.78 g) in anhydrous diethyl ether (12.5 ml) was treated with a solution of methanesulphonic acid (2.40 g) in anhydrous diethyl ether (12.5 ml), stirred and cooled. The solid precipitate was removed by filtration, washed with cold anhydrous diethyl ether and dried at 0.05 mm Hg for 2 hours, to give 1-(3,5-bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne methanesulphonate (11.61 g), m.p. 164°-165° C., in the form of a white powder which had the elementary analysis C: 51.3%; H: 5.49%; N: 2.60% (C21H27F6NO3S requires C: 51.73%; H: 5.58%; N: 2.87%).

Quelle