反应详情

To a solution of 2-(benzyloxy)-3,3,3-trifluoro-2-methylpropanoic acid (Int. D) (0.709 g, 2.85 mmol) in DMF (15 ml) was added HATU (1.303 g, 3.43 mmol) followed by DIPEA (0.598 ml, 3.43 mmol). After 30 mins, tert-butyl 2-(hydrazinecarbonyl)-6-methoxy-5-(trifluoromethyl)pyridin-3-ylcarbamate (Int. C) (1 g, 2.85 mmol) was added and the reaction mixture was stirred at RT for 3 h. The mixture was poured into water and the product extracted with EtOAc. The organic portion was washed with 1 MHCl, brine, dried (MgSO4) and concentrated in vacuo. Purification by chromatography on silica eluting with 0% to 50% EtOAc in iso-hexane afforded the title compound:

1. extractionthe product extracted with EtOAc
2. washThe organic portion was washed with 1 MHCl, brine
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo
5. customPurification by chromatography on silica eluting with 0% to 50% EtOAc in iso-hexane