2-(4-Amino-3-chloro-5-trifluoromethylphenyl)-2-tert-butylaminoethanol → 2-(4-Amino-3-chloro-5-trifluoromethyl-phenyl)-2-tert-butylaminoethanol hydrochloride

関与物質

反応手順

1.0 g of 2-(4-amino-3-chloro-5-trifluoromethylphenyl)-2-tert-butylaminoethanol was dissolved in 20 ml of diethyl ether and filtered. Saturated solution of hydrogen chloride in isopropanol was added dropwise and acidified to pH=2. The precipitate was collected by filtration, washed with anhydrous ether, and dried to give crude 2-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-2-tert-butylaminoethanol hydrochloride. The crude product was dissolved in absolute ethanol at a ratio of 1:5 w/v. Filtered, anhydrous ether was added dropwise until small amount of crystals was precipitated. Lyophilized and filtered to give 2-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-2-tert-butylaminoethanol hydrochloride. Yield 80–90%; melting point 205–206° C. (dec). 1H-NMR (DMSO-d6) δ:1.24 (9H, s), 3.77(2H, d), 4.42–4.44(1H, m), 7.72(1H, s), 7.87(1H, s).

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