反应详情

温度

90 °C

In a 50 ml round-bottomed flask 2-[(3-ethyl-1,3-dihydro-2-benzofuran-4-yl)oxy]-5-nitropyridine (Intermediate 107, 97.6 mg) was dissolved in ethanol (10 ml) to give a pale yellow solution. Pd/C (26.1 mg, 0.245 mmol) and hydrazine hydrate (12.29 mg, 0.245 mmol) were added. The reaction mixture was stirred at 90° C. After 45 minutes, the reaction was completed. The reaction mixture was filtered and the organic phase was evaporated under vacuum affording the crude product which was charged on a 2 g SCX cartridge. It was then flushed with 15 ml of methanol followed by 15 ml of a 2M solution of ammonia in methanol. The ammonia eluate was evaporated under vacuum affording nothing. The methanol eluate was then evaporated under vacuum to afford the title compound as a colourless oil.

1. customto give a pale yellow solution
2. filtrationThe reaction mixture was filtered
3. customthe organic phase was evaporated under vacuum
4. customaffording the crude product which
5. additionwas charged on a 2 g SCX cartridge
6. customIt was then flushed with 15 ml of methanol
7. customThe ammonia eluate was evaporated under vacuum
8. customaffording nothing
9. customThe methanol eluate was then evaporated under vacuum