반응 #96204

반응 방정식

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

수율 95.4%

용매

diethyl ether

diethyl ether

반응 조건

후처리

1. 1
   온도cooled
2. 2
   기타The solid precipitate was removed by filtration
3. 3
   세척washed with cold anhydrous diethyl ether
4. 4
   기타dried at 0.05 mm Hg for 2 hours

실험 절차

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%).

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