反应详情

To 3-[{4-[(4-acetyl-3-hydroxy-2-methyl-phenylamino)-methyl]-phenyl}-(tetrahydro-pyran-2-yloxy)-methyl]-benzonitrile (538 mg, 1.1 mmol) in MeOH (5 mL) is added conc. HCl (0.33 mL). The reaction mixture is stirred at RT for 6 h. The reaction mixture is concentrated and the residue partitioned between saturated aqueous NaHCO3 and EtOAc. The organic layer is separated and the aqueous extracted with EtOAc (2×). The organic layers are combined, washed with brine, dried over Na2SO4, and concentrated. The residue is purified by flash column chromatography using 40% EtOAc/hexane as eluent. Obtained is the title compound as yellow foam (305 mg, 72%). LC-MS (m/e): 385 (M−1).

1. concentrationThe reaction mixture is concentrated
2. customthe residue partitioned between saturated aqueous NaHCO3 and EtOAc
3. customThe organic layer is separated
4. extractionthe aqueous extracted with EtOAc (2×)
5. washwashed with brine
6. dry with materialdried over Na2SO4
7. concentrationconcentrated
8. customThe residue is purified by flash column chromatography
9. customObtained