反応 #96204

反応方程式

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

収率 95.4%

溶媒

diethyl ether

diethyl ether

反応条件

後処理

1. 1
   温度cooled
2. 2
   その他The solid precipitate was removed by filtration
3. 3
   洗浄washed with cold anhydrous diethyl ether
4. 4
   その他dried at 0.05 mm Hg for 2 hours

実験手順

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%).

出典