Reaktion #718032

Reaktionsgleichung

Intermediate 90b

(R)-3-(6-Fluoro-[1,2,4]triazolo[4,3-a]pyridin-3-yl)-pyrrolidine-1-carboxylic acid tert-butyl ester

TFA

→

6-Fluoro-3-(R)-pyrrolidin-3-yl-[1,2,4]triazolo[4,3-a]pyridine

Lösungsmittel

DCM

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux for 45 min
2. 2
   EinengenThe cooled solution was concentrated in vacuo
3. 3
   Waschenwashed with MeOH (50 mL)
4. 4
   WaschenThe product was eluted with 2M NH3 in MeOH
5. 5
   Einengenconcentration in vacuo
6. 6
   workup.WAITleft the title compound as a pale yellow solid (225 mg, >99%)

Vorschrift

A mixture of Intermediate 90b (335 mg, 1.09 mmol) and TFA (0.812 mL, 10.9 mmol) in DCM (5 mL) was stirred at reflux for 45 min. The cooled solution was concentrated in vacuo, redissloved in MeOH (2 mL), applied to an SCX-2 cartridge (10 g) and washed with MeOH (50 mL). The product was eluted with 2M NH3 in MeOH; concentration in vacuo left the title compound as a pale yellow solid (225 mg, >99%). LCMS (Method 3): Rt 0.44 min, m/z 207 [MH+].

Quelle