反应详情

A solution of the 22-4 (0.141 g, 0.268 mmol) in 25 mL absolute EtOH was treated with 10% Pd—C (0.015 g, 10% by wt) at room temperature under an argon atmosphere. Then ammonium formate (0.101 g, 1.61 mmol) was added and the heterogeneous mixture was refluxed for 30 minutes. The reaction was >50% complete (by ms). At this point, more Pd—C (0.008 g, 5% by wt) and NH4CO2 (0.050 g, 0.80 mmol) were added and the mixture refluxed for an additional 30. minutes (reaction complete by ms). The solution was then filtered through a Celite plug, washed with EtOH (75 mL), and concentrated in vacuo to afford 0.130 g 22-5.

1. temperaturethe heterogeneous mixture was refluxed for 30 minutes
2. temperaturethe mixture refluxed for an additional 30
3. customminutes (reaction complete by ms)
4. filtrationThe solution was then filtered through a Celite plug
5. washwashed with EtOH (75 mL)
6. concentrationconcentrated in vacuo