Реакция #674296

Уравнение реакции

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

Выход 61.0%

Растворители

formic acid

Условия реакции

Обработка

1. 1
   ДругоеThe solution was sonicated at room temperature for 1.0 h
2. 2
   Концентрированиеconcentrated by evaporation in vacuo
3. 3
   Другоеto give the residue
4. 4
   Другоеevaporated again
5. 5
   workup.ADDITIONEther (10 mL) was added
6. 6
   ФильтрацияThe solid was collected by filtration
7. 7
   Промывкаwashed with ether (10 mL)
8. 8
   Другоеdried under high vacuum

Методика

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.

Источник