反应详情

To a solution of ethyl [4-({(2-cyclopropylethyl)[4′-(trifluoromethyl)-1,1′-biphenyl-3-yl]amino}sulfonyl)-2-methylphenoxy]acetate (156 mg, 0.28 mmol) in MeOH (2 mL) and THF (2 mL) at room temperature was added 2M NaOH aq. (1 mL, 2 mmol). The resultant mixture was stirred for 2 h. The solvents were removed in vacuo and the residue was partitioned between EtOAc (2×20 mL) and 2M HCl (20 mL). The organic solution was dried (MgSO4) and the solvent was removed in vacuo. Purification by SPE (5 g aminopropyl cartridge), loading crude material in CH2Cl2 and then washing with MeOH, prior to eluting with 5% NH3 in MeOH. The 5% NH3 in MeOH extract was concentrated in vacuo and the residue was partitioned between CH2Cl2 (20 mL) and 2M HCl (2 mL). The organic solution was dried (MgSO4) and the solvent was removed in vacuo affording the title compound as a white solid (64.4 mg).

1. customThe solvents were removed in vacuo
2. customthe residue was partitioned between EtOAc (2×20 mL) and 2M HCl (20 mL)
3. dry with materialThe organic solution was dried (MgSO4)
4. customthe solvent was removed in vacuo
5. customPurification by SPE (5 g aminopropyl cartridge)
6. washwashing with MeOH
7. washto eluting with 5% NH3 in MeOH
8. extractionThe 5% NH3 in MeOH extract
9. concentrationwas concentrated in vacuo
10. customthe residue was partitioned between CH2Cl2 (20 mL) and 2M HCl (2 mL)
11. dry with materialThe organic solution was dried (MgSO4)
12. customthe solvent was removed in vacuo