Diethylethanolamine → 2-Diethylaminoethyl 2-[4-(4-chlorophenyl)benzyloxy]-3,3,3-trifluoro-2-trifluoromethylpropionate hydrochloride
反応式
[CH2:1]([N:3]([CH2:7][CH3:8])[CH2:4][CH2:5][OH:6])[CH3:2].[Cl:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH:35]=[CH:34][C:19]([CH2:20][O:21][C:22]([C:30]([F:33])([F:32])[F:31])([C:26]([F:29])([F:28])[F:27])[C:23](Cl)=[O:24])=[CH:18][CH:17]=2)=[CH:12][CH:11]=1>N1C=CC=CC=1>[ClH:9].[Cl:9][C:10]1[CH:15]=[CH:14][C:13]([C:16]2[CH:17]=[CH:18][C:19]([CH2:20][O:21][C:22]([C:26]([F:27])([F:28])[F:29])([C:30]([F:31])([F:32])[F:33])[C:23]([O:6][CH2:5][CH2:4][N:3]([CH2:7][CH3:8])[CH2:1][CH3:2])=[O:24])=[CH:34][CH:35]=2)=[CH:12][CH:11]=1参加物
4
実験手順
A mixture of 2-diethylaminoethanol (814 mg.) and pyridine (10 ml.) is added at 0° C. to 2-[4-(4-chlorophenyl)benzyloxy]-3,3,3-trifluoro-2-trifluoromethylpropionyl chloride (3.07 g.). The mixture is stirred at room temperature until the acid chloride dissolves, and the solution is stored at 0° C. for 2 days. The mixture is filtered and the filtrate evaporated. The residue is triturated with ether and combined with the solid previously filtered off. The combined solids are crystallised from dioxan-ether to give 2-diethylaminoethyl 2-[4-(4-chlorophenyl)benzyloxy]-3,3,3-trifluoro-2-trifluoromethylpropionate hydrochloride (2.2 g.), m.p. 139°-140° C. (decomposition).