反应详情

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).

1. filtrationfiltered
2. additionSaturated solution of hydrogen chloride in isopropanol was added dropwise
3. filtrationThe precipitate was collected by filtration
4. washwashed with anhydrous ether
5. customdried
6. customto give crude 2-(4-amino-3-chloro-5-trifluoromethyl-phenyl)-2-tert-butylaminoethanol hydrochloride
7. filtrationFiltered
8. additionanhydrous ether was added dropwise until small amount of crystals
9. customwas precipitated
10. filtrationLyophilized and filtered