反应详情

A mixture of 0.5 g (1.4 mmoles) of 58 , 20 ml of ethanol, 10 ml of methylene chloride and 0.4 g of 10% Pd/C catalyst was hydrogenated with 70 psi hydrogen for 3 h at room temperature. The crude reaction slurry was filtered through Celite and evaporated to dryness. The residue was purified by HPLC (10% EtOAc-Hexane, 25% EtOAc-Hexane). The first fraction was 300 mg (60%) as a white solid, mp 99-100° C. Proton NMR showed this was a trans isomer. The second fraction gave 200 mg of solid which was impure cis isomer.

1. customThe crude reaction slurry
2. filtrationwas filtered through Celite
3. customevaporated to dryness
4. customThe residue was purified by HPLC (10% EtOAc-Hexane, 25% EtOAc-Hexane)