反应详情

A sealed tube containing tert-butyl (3R)-3-(hydroxymethyl)-4-{2-hydroxy-2-[(3S)-3-methyl-1-oxo-3,4-dihydro-1H-isochromen-6-yl]propyl}piperazine-1-carboxylate (175 mg, 0.403 mmol) and cyanomethylenetributylphosphorane (117 mg, 0.483 mmol) dissolved in anhydrous benzene (3 mL) was degassed twice with nitrogen and then heated using a microwave to 135° C. for 2.5 hours. The reaction was allowed to cool and the crude mixture was concentrated and purified on MPLC (30-75% EtOAc/Hex) to afford the minor isomer as the faster eluting peak and the major isomer as the slower eluting peak: Major, slower eluting isomer: LC-MS: (M+1)+417.

1. customwas degassed twice with nitrogen
2. temperatureheated
3. customto 135° C.
4. customfor 2.5 hours
5. temperatureto cool
6. concentrationthe crude mixture was concentrated
7. custompurified on MPLC (30-75% EtOAc/Hex)
8. customto afford the minor isomer as the
9. washfaster eluting peak
10. washthe major isomer as the slower eluting peak
11. washMajor, slower eluting isomer