Isethionic Acid → 1-(3,5-Bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne 2-hydroxyethanesulphonate
反応式
[F:1][C:2]([F:27])([F:26])[C:3]1[CH:4]=[C:5]([C:13]#[C:14][CH2:15][N:16]2[CH2:21][CH2:20][CH:19]([C:22]([CH3:25])([CH3:24])[CH3:23])[CH2:18][CH2:17]2)[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.[OH:28][CH2:29][CH2:30][S:31]([OH:34])(=[O:33])=[O:32]>C(OCC)(=O)C>[OH:28][CH2:29][CH2:30][S:31]([OH:34])(=[O:33])=[O:32].[F:12][C:9]([F:10])([F:11])[C:7]1[CH:6]=[C:5]([C:13]#[C:14][CH2:15][N:16]2[CH2:17][CH2:18][CH:19]([C:22]([CH3:23])([CH3:24])[CH3:25])[CH2:20][CH2:21]2)[CH:4]=[C:3]([C:2]([F:26])([F:27])[F:1])[CH:8]=1参加物
4
実験手順
A solution of 1-(3,5-bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne (6.1 g) in ethyl acetate (20 ml) was treated with 2-hydroxyethanesulphonic acid (2.19 g) in ethyl acetate (20 ml). Evaporation of the solvent gave a waxy solid, m.p. 107°-109° C., which was recrystallised from a mixture of ethyl acetate and diethyl ether to give 1-(3,5-bistrifluoromethylphenyl)-3-(4-tert-butylpiperidino)prop-1-yne 2-hydroxyethanesulphonate (containing 0.23 mole of water of crystallization) (5.61 g), m.p. 118°-119° C., in the form of a white crystalline solid which had the elementary analysis C: 50.3%; H: 6.05%; N: 2.68%; H2O: 0.8% (C22H29F6NO4S. 0.23 H2O requires C: 50.64%; H: 5.65%; N: 2.68%; H2O: 0.8%).