反应详情

Crude HCl salt of 101 was mixed with 201.8 mg (0.1896 mmol) of palladium on charcoal (10%) in 15 mL of methanol. The mixture was subjected to hydrogen atmosphere at 50 psi on a Parr apparatus at room temperature. After overnight, another 200.9 mg of catalyst was needed. After overnight, reaction was completed and the insolubles was filtered off through glass fiber filter paper. The filtrate was concentrated to yield 254.6 mg (quant.) of product 102 as HCl salt: 1H NMR (400 MHz, CDCl3): δ 2.89 (s, 6H), 3.06 (s, 3H), 3.21 (t, J=6.6, 2H), 3.93 (t, J=6.6, 2H), 4.25 (s, 2H).

1. waitAfter overnight
2. customreaction
3. filtrationthe insolubles was filtered off through glass fiber
4. filtrationfilter paper
5. concentrationThe filtrate was concentrated