反应详情

温度

50 °C

(R)-3-(N,N-Dibenzylamino)-8-fluoro-5-methoxy-3,4-dihydro-2H-1-benzopyran (13.0 g, 34.4 mmol) was dissolved in 265 mL methanol and 115 mL THF. To this was 10% Pd/C (4 g) and ammonium formate (51.5 g, 0.817 mol) added. The reaction was heated to 50° C. for 2.5 h. The reaction was filtered and the solvent was removed in vacuo, the remains were taken into a 2 M solution of NaOH and then extracted twice with ether. The combined ether portions were treated with brine, dried (Na2SO4), filtered, and the solvent removed in vacuo to give 6.2 g (91% yield) of the title compound as a clear oil. [α]21D =-15.3° (C=1 CHCl3) GC-MS (70 eV) M=197 (51%).

1. filtrationThe reaction was filtered
2. customthe solvent was removed in vacuo
3. extractionextracted twice with ether
4. additionThe combined ether portions were treated with brine
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. customthe solvent removed in vacuo