反应详情

A suspension of 5a (0.3 g, 1.03 mmol) and catalyst (10% palladium on carbon, 0.8 g, 50% wet) in methanol (25 mL) was placed in a Parr shaker bottle. The system was vacuumed and flushed with nitrogen. The procedure was repeated three times. The mixture was then shaken at room temperature overnight under 40 psi hydrogen atmosphere. The system was then vacuumed again and flushed with nitrogen. The procedure was repeated three times. The catalyst was filtered under vacuum and washed with methanol (2×10 mL). The filtrate and washings were combined and concentrated under reduced pressure to provide 6a (186 mg, 90%). The crude product was used directly without purification. m/z (ESI): 201 [C11H24N2O+H]+.

1. customflushed with nitrogen
2. customflushed with nitrogen
3. filtrationThe catalyst was filtered under vacuum
4. washwashed with methanol (2×10 mL)
5. concentrationconcentrated under reduced pressure