反应详情

To a solution of 41 (2.5 g, 5.48 mmol) in MeOH (200 mL) was added CSA (127 mg, 0.548 mmol) and the reaction mixture was heated to reflux for 5 hours. It was then cooled to RT and solid NaHCO3 was added. The mixture was filtered and the filtrate was concentrated to dryness. The residual solid was dissolved in DCM, washed with water, dried over Na2SO4, filtered and concentrated. The resultant solid was triturated with Et2O to afford 42 (1.8 g, 74% yield) which was used without any further purification. MS (m/z): 445.1 (M+H).

1. temperaturethe reaction mixture was heated
2. temperatureto reflux for 5 hours
3. filtrationThe mixture was filtered
4. concentrationthe filtrate was concentrated to dryness
5. dissolutionThe residual solid was dissolved in DCM
6. washwashed with water
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated
10. customThe resultant solid was triturated with Et2O