反应详情

A mixture of 750 mg of the crude product of Step F in MeOH (30 mL), concentrated aqueous HCl (1 mL), and 100 mg of moist Pearlman's catalyst were shaken under 1 atm. H2 for 24 hours. The reaction was incomplete so 100 mg more of the catalyst was added and the reaction was shaken as described above for an additional 24 hours. Filtration, concentration, and extraction from dilute NH4OH with EtOAc followed by drying (Na2SO4), concentration, and purification (SiO2, 5% MeOH/EtOAc) gave 250 mg of the title compound as a solid.

1. additionwas added
2. stirringthe reaction was shaken
3. customas described above for an additional 24 hours
4. filtrationFiltration, concentration, and extraction from dilute NH4OH with EtOAc
5. customby drying
6. concentration(Na2SO4), concentration, and purification (SiO2, 5% MeOH/EtOAc)