反应详情

A mixture of 3-[4-(benzyloxy)-3-chlorophenyl]-1-cyclopentylpropan-1-one (48 g, 0.140 mole), from Step 1, and 10% palladium-on-carbon (11.52 g of 50 wt % wet, 0.005 mol, 3.5 mole %) in ethyl acetate (500 mL) was degassed and purged with hydrogen three times. The reaction was stirred with 1 atm H2 for 4 h, resulting in complete conversion. The mixture was filtered through a fine fritted glass funnel and the filtrate concentrated in vacuo, affording a yellow oil which crystallized on cooling. This material was recrystallized from two parts of isopropyl ether, affording 22 g (62%) of the title product. mp 88-90° C.

1. custompurged with hydrogen three times
2. customresulting in complete conversion
3. filtrationThe mixture was filtered through a fine fritted glass funnel
4. concentrationthe filtrate concentrated in vacuo
5. customaffording a yellow oil which
6. customcrystallized
7. temperatureon cooling
8. customThis material was recrystallized from two parts of isopropyl ether