反应详情

Add TFA (0.6 mL, 7.94 mmol) to a solution of 3′-[4-(Acetylamino-methyl)-phenyl]-2,3,5,6-tetrahydro-[1,2′]bipyrazinyl-4-carboxylic acid tert-butyl ester (650 mg, 1.58 mmol) in DCM (6.5 mL) and maintain stirring for 3 hr. Concentrate material to dryness. Redissolve in DCM (10 mL) and add TFA (1.2 mL). Heat reaction mixture at 40° C. for 3 hr. Purify the mixture by SCX-2® ion exchange chromatography, eluting with 2 M NH3 in MeOH to give the title compound as a yellow oil (454 mg, 92%). 1H-NMR (400 MHz, CDCl3) δ 8.14 (d, 1H), 8.08 (d, 1H), 7.90 (d, 2H), 7.36 (d, 2H), 5.81 (bs, 1H), 4.49 (d, 2H), 3.17 (m, 4H), 2.88 (m, 4H), 2.06 (s, 3H).

1. temperaturemaintain
2. temperatureHeat
3. customreaction mixture at 40° C. for 3 hr
4. customPurify the mixture by SCX-2® ion exchange chromatography
5. washeluting with 2 M NH3 in MeOH