反应详情

Lidlar's catalyst (20 mg) was added to compound 30 (0.10 g, 0.20 mmol), and was then suspended in ethanol (5 ml). Air was removed from the flask by flushing with nitrogen several times. The nitrogen was then removed and replaced with hydrogen. The mixture was stirred for 5 hours, and then filtered through Celite. Fresh Lidlar's catalyst (20 mg) was added to the filtrate. The flask was flushed with nitrogen and then hydrogen as previously, and the reaction was left stirring for another 3 hours. The reaction mixture was filtered through Celite. The solvent was evaporated and the concentrated solution was purified by column chromatography (MeOH/DCM 2%→10%) which gave the title product as a white solid (0.065 g, 70%). Rf: 0.3 in DCM/MeOH 90:10.

1. customAir was removed from the flask
2. customby flushing with nitrogen several times
3. customThe nitrogen was then removed
4. filtrationfiltered through Celite
5. additionFresh Lidlar's catalyst (20 mg) was added to the filtrate
6. customThe flask was flushed with nitrogen
7. waithydrogen as previously, and the reaction was left
8. stirringstirring for another 3 hours
9. filtrationThe reaction mixture was filtered through Celite
10. customThe solvent was evaporated
11. customthe concentrated solution was purified by column chromatography (MeOH/DCM 2%→10%) which