反应详情

To a solution of 9 (1.0 g, 3.78 mmol) in anhydrous methanol (90 mL) was added 10%Pd/C (150 mg) suspended in anhydrous methanol (15 mL) followed by ammonium formate (1.10 g, 17.4 mmol). The reaction mixture was stirred for 1 h, filtered through celite and the methanol removed. The residue was taken up in CH2Cl2/H2O and extracted with CH2Cl2 (3×). The combined organic layers were dried over Na2SO4 and evaporated to afford 10 (595 mg, 67%) as a brown solid which was used without further purification; 1H NMR (CDCl3): δ7.21 (1H, s), 7.06 (1H, d), 6.72 (1H, d), 4.01 (3H, s), 3.90 (3H, s), 3.88 (3H, s).

1. filtrationfiltered through celite
2. customthe methanol removed
3. extractionextracted with CH2Cl2 (3×)
4. dry with materialThe combined organic layers were dried over Na2SO4
5. customevaporated