反应详情

温度

130 °C

Intermediate (1c) (540 mg, 1.9 mmol) was dissolved in MeOH (927 μL, 22.9 mmol). Water (1.84 mL, 102 mmol) was added, followed by the addition of KOH (1.1 g, 18.8 mmol). The reaction was refluxed at 130° C. for 3 hours. The mixture was diluted to 250 mL with saturated ammonium chloride, then washed (2×100 mL hexane). The remaining aqueous emulsion was washed (2×250 mL EtOAc). The EtOAc layers were combined, washed with 50 mL saturated aqueous NaCl, dried over Na2SO4, filtered and concentrated to yield intermediate (1d) as a brownish-yellow solid (290 mg).

1. washwashed (2×100 mL hexane)
2. washThe remaining aqueous emulsion was washed (2×250 mL EtOAc)
3. washwashed with 50 mL saturated aqueous NaCl
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated