反应详情

To a 35° C. mixture of 50 g of 2-methyl-5-nitrobenzofuran, ethanol (250 mL), THF (250 mL) and wet 10% Pd/C (4 g) was added ammonium formate (53.4 g, 0.85 mol) over 50 min. After an additional 4 h, the reaction was cooled to room temperature and filtered through Celite. The filtrate was concentrated and the residue was taken up in methyl t-butyl ether (415 mL). This mixture was filtered and a solution of oxalic acid (25.4 g) in methanol (80 mL) was added dropwise. The precipitate was stirred for 2 h, collected, washed with methanol/TBME and dried to provide 2-methyl-5-benzofuranamine oxalate.

1. filtrationfiltered through Celite
2. concentrationThe filtrate was concentrated
3. filtrationThis mixture was filtered
4. additiona solution of oxalic acid (25.4 g) in methanol (80 mL) was added dropwise
5. customcollected
6. washwashed with methanol/TBME
7. customdried