Reaktion #674296

Reaktionsgleichung

tert-Butyl 6-(4-(6-amino-5-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)pyridin-3-yl)-1H-pyrazol-1-yl)-2-azaspiro[3.3]heptane-2-carboxylate

Toluene

→

(±)-5-(1-(2-azaspiro[3.3]heptan-6-yl)-1H-pyrazol-4-yl)-3-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)pyridin-2-amine formate

Ausbeute 61.0%

Lösungsmittel

formic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solution was sonicated at room temperature for 1.0 h
2. 2
   Einengenconcentrated by evaporation in vacuo
3. 3
   Sonstigeto give the residue
4. 4
   Sonstigeevaporated again
5. 5
   workup.ADDITIONEther (10 mL) was added
6. 6
   FiltrationThe solid was collected by filtration
7. 7
   Waschenwashed with ether (10 mL)
8. 8
   Sonstigedried under high vacuum

Vorschrift

tert-Butyl 6-(4-(6-amino-5-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)pyridin-3-yl)-1H-pyrazol-1-yl)-2-azaspiro[3.3]heptane-2-carboxylate (53 mg, 0.094 mmol) was dissolved in formic acid (3 mL). The solution was sonicated at room temperature for 1.0 h and then concentrated by evaporation in vacuo to give the residue. Toluene (2×5 mL) was added and evaporated again. Ether (10 mL) was added and the mixture was stirred at room temperature for 1.0 h. The solid was collected by filtration, washed with ether (10 mL) and then dried under high vacuum to afford (±)-5-(1-(2-azaspiro[3.3]heptan-6-yl)-1H-pyrazol-4-yl)-3-(1-(2,6-dichloro-3-fluorophenyl)ethoxy)pyridin-2-amine formate (29 mg, 61%) as an off-white solid.

Quelle