反应详情

温度

70 °C

To a solution of ethyl 2-{4-[(butyl{6-[4-(trifluoromethyl)phenyl]pyridin-2-yl}amino)methyl]-2-methylphenoxy}-2-methylpropanoate (45 mg, 0.085 mmol) in methanol (1.5 mL) and tetrahydrofuran (1.5 mL) was added 2M NaOH aq. (1 mL). The resulting mixture was heated to 70° C. for 1 h and then stirred at room temperature for 18 h, before heating to 70° C. for a further 4 h. The reaction mixture was allowed to attain room temperature and the solvents removed in vacuo. The residue was acidified with 2M HCl and extracted with EtOAc (2×10 mL). The organic solution was dried (MgSO4) and the solvents removed in vacuo. Purification by aminopropyl SPE (5 g) conditioning the cartridge, loading the compound and washing with methanol before eluting using 10% NH3 in methanol. Evaporation of the methanolic ammonia yielded a white solid, which was treated with 1 M HCl (5 mL) and then extracted into CH2Cl2 (20 mL). The organic extract was dried (Na2SO4) and the solvent removed in vacuo to afford the title compound as a colourless oil (19 mg).

1. temperaturebefore heating to 70° C. for a further 4 h
2. customto attain room temperature
3. customthe solvents removed in vacuo
4. extractionextracted with EtOAc (2×10 mL)
5. dry with materialThe organic solution was dried (MgSO4)
6. customthe solvents removed in vacuo
7. customPurification by aminopropyl SPE (5 g) conditioning the cartridge
8. washwashing with methanol
9. washbefore eluting
10. customEvaporation of the methanolic ammonia
11. customyielded a white solid, which
12. extractionextracted into CH2Cl2 (20 mL)
13. extractionThe organic extract
14. dry with materialwas dried (Na2SO4)
15. customthe solvent removed in vacuo