反应详情

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, redissolved 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+].

1. temperatureat reflux for 45 min
2. concentrationThe cooled solution was concentrated in vacuo
3. dissolutionredissolved in MeOH (2 mL)
4. washwashed with MeOH (50 mL)
5. washThe product was eluted with 2M NH3 in MeOH
6. concentrationconcentration in vacuo
7. waitleft the title compound as a pale yellow solid (225 mg, >99%)