Reaktion #1592035

Reaktionsgleichung

tert-Butyl [(1S,2R)-2-({6-carbamoyl-5-[(4,6-dimethylpyridin-2-yl)amino]pyridin-3-yl]amino)cyclohexyl}carbamate

hydrochloric acid

hydrochloric acid

→

5-{[(1R,2S)-2-aminocyclohexyl]amino}-3-[(4,6-dimethylpyridin-2-yl)amino]pyridine-2-carboxamide hydrochloric acid salt

Lösungsmittel

—

hexanes

dioxane

—

hexanes

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationfiltered
2. 2
   SonstigeThe collected solids were dried in a nitrogen bag
3. 3
   workup.ADDITIONThe solids were diluted with dioxane (140 mL)
4. 4
   workup.WAITAfter 1 hour
5. 5
   Filtrationfiltered
6. 6
   Waschenwashed with hexanes (2×150 mL)
7. 7
   SonstigeThe isolated solids were dried under reduced pressure
8. 8
   Filtrationthe mixture was filtered
9. 9
   Sonstigedried in a nitrogen bag

Vorschrift

tert-Butyl [(1S,2R)-2-({6-carbamoyl-5-[(4,6-dimethylpyridin-2-yl)amino]pyridin-3-yl]amino)cyclohexyl}carbamate (22.5 g, 49.5 mmol) was diluted with dioxane (140 mL). To this solution was added hydrochloric acid (4.0 M in dioxane, 62 mL, 250 mmol). After 30 minutes, the reaction mixture was diluted with hexanes (400 mL) and filtered. The collected solids were dried in a nitrogen bag. The solids were diluted with dioxane (140 mL) followed by hydrochloric acid (4.0 M in dioxane, 62 mL, 250 mmol). After 1 hour, the reaction mixture was diluted with hexanes (400 mL), filtered, and washed with hexanes (2×150 mL). The isolated solids were dried under reduced pressure, and then suspended in dichloromethane (300 mL). After stirring for 3 hours, the mixture was filtered and dried in a nitrogen bag to afford 5-{[(1R,2S)-2-aminocyclohexyl]amino}-3-[(4,6-dimethylpyridin-2-yl)amino]pyridine-2-carboxamide hydrochloric acid salt.

Quelle