Hydrochloric Acid → (5S)-4-(4,4-Difluorocyclohexyl)-3-{(S)-fluoro[4-(trifluoromethyl)phenyl]methyl}-2-(1-{5-[3-hydroxy-2-(hydroxymethyl)propoxy]pyrimidin-2-yl}piperidin-4-yl)-7,7-dimethyl-5,6,7,8-tetrahydr oquinolin-5-ol dihydrochloride

Temperatur

60 °C

To a solution of 0.70 g (0.95 mmol) of (5S)-4-(4,4-Difluorocyclohexyl)-3-{(S)-fluoro[4-(trifluoromethyl)phenyl]methyl}-2-(1-{5-[3-hydroxy-2-(hydroxymethyl)propoxy]pyrimidin-2-yl}piperidin-4-yl)-7,7-dimethyl-5,6,7,8-tetrahydroquinolin-5-ol, which was prepared by a method similar to that of Reference Example 22, in 4.8 ml of ethyl acetate, 0.17 ml (2.0 mmol) of 35% hydrochloric acid was added dropwise with stirring at 60° C. Then, the reaction mixture was cooled to 20° C. and stirred for 3 hours. The precipitated solid was obtained by filtration, washed with 5 ml of ethyl acetate twice and then dried under reduced pressure at 60° C. to provide 659 mg of the title compound as a white powder (yield: 86%).

1. temperatureThen, the reaction mixture was cooled to 20° C.
2. stirringstirred for 3 hours
3. customThe precipitated solid was obtained by filtration
4. washwashed with 5 ml of ethyl acetate twice
5. customdried under reduced pressure at 60° C.

ORD-Eintrag

ord-ae51212294cd40648f31b0fffa767302

Quelldatensatz

uspto-grants-2016_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09321747B2