Reaktion #679643

Reaktionsgleichung

tert-butyl 4-((4-((2-(1-amino-1-oxopropan-2-yl)phenyl)ethynyl)-5-(trifluoromethyl)pyrimidin-2-yl)amino)-1H-pyrazole-1-carboxylate

TFA

→

title compound

2-(2-((2-((1H-Pyrazol-4-yl)amino)-5-(trifluoromethyl)pyrimidin-4-yl)ethynyl)phenyl)propanamide

Lösungsmittel

DCM

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe mixture was concentrated under reduced pressure
2. 2
   workup.ADDITIONdiluted with water (50 mL)
3. 3
   Extraktionbefore extracting with DCM (2×50 mL) and EtOAc (50 mL)
4. 4
   EinengenThe combined organic residues were concentrated
5. 5
   Sonstigepurified
6. 6
   Sonstige50-100% EtOAc in petroleum benzine 40-60° C.

Vorschrift

A mixture of tert-butyl 4-((4-((2-(1-amino-1-oxopropan-2-yl)phenyl)ethynyl)-5-(trifluoromethyl)pyrimidin-2-yl)amino)-1H-pyrazole-1-carboxylate A62 (0.31 g, 0.62 mmol) and TFA (0.90 mL, 12 mmol) in DCM (3.0 mL) was stirred for 2 hours at room temperature. The mixture was concentrated under reduced pressure and diluted with water (50 mL) before extracting with DCM (2×50 mL) and EtOAc (50 mL). The combined organic residues were concentrated and purified using silica gel column chromatography (50-100% EtOAc in petroleum benzine 40-60° C. then 0-10% MeOH in EtOAc) to give the title compound A63 (0.211 g, 85%). LCMS-D: rt 3.162 min; m/z 401.2 [M+H]+.

Quelle