反应详情

To a degassed solution of 3-(1-trityl-1H-imidazol-4-yl)but-2-enoic acid ethyl ester (5 g, 11.8 mmol) in ethanol (100 mL) in a Parr bottle is added 5% palladium on carbon (0.5 g). The bottle is purged with nitrogen, evacuated, and hydrogen gas (15 psi) added. The bottle is placed upon a Parr hydrogenation apparatus and shaken for 18 h. The hydrogen is evacuated and the bottle purged with nitrogen gas. The reaction mixture is then filtered through diatomaceous earth and the clear liquid solution collected and the solvent removed in vacuo to give the crude oil, which is subject to flash chromatography (silica gel) eluting with MeOH:CH2Cl2 to yield the desired compound.

1. customThe bottle is purged with nitrogen
2. customevacuated
3. additionhydrogen gas (15 psi) added
4. customThe hydrogen is evacuated
5. customthe bottle purged with nitrogen gas
6. filtrationThe reaction mixture is then filtered through diatomaceous earth
7. customthe clear liquid solution collected
8. customthe solvent removed in vacuo
9. customto give the crude oil, which
10. washeluting with MeOH