反应详情

Compound (i) (736 mg, 3.06 mmol) was dissolved in MeOH (15 mL) at RT and this solution degassed with N2. Palladium on carbon (10%) (25 mg) was suspended in water/MeOH (0.5 mL/2 mL) and added to the substrate solution. The mixture was again degassed with N2 and then vacuum/flushed with H2. The mixture was stirred under a H2 balloon overnight at RT. The mixture was filtered through celite, washed with MeOH and the filtrate evaporated to dryness to afford a clear oil which was placed under high vacuum for 1 h to afford the desired product (ii), 620 mg. 1H NMR (400 MHz, CDCl3) δ 6.88 (d, J=8.3 Hz, 2H), 6.60 (d, J=8.3 Hz, 2H), 3.64 (s, 3H), 2.74 (s, 2H), 1.15 (s, 6H).

1. customthis solution degassed with N2
2. additionadded to the substrate solution
3. customThe mixture was again degassed with N2
4. customvacuum/flushed with H2
5. filtrationThe mixture was filtered through celite
6. washwashed with MeOH
7. customthe filtrate evaporated to dryness
8. customto afford a clear oil which
9. waitwas placed under high vacuum for 1 h