反应详情

温度

115 °C

A suspension of 16B (1.2 g, 4.7 mmol) in a mixture of ethanol (30 mL), water (5 mL), and acetic acid (3.3 mL, 5.8 mmol) was heated by a 115° C. oil bath. Iron powder (1.80 g, 32.2 mmol) was added portionwise over 1 h. The reaction mixture was cooled to rt, filtered, and washed with ethyl acetate. Sodium bicarbonate solution was added until it was basic. The reaction mixture was extracted with ethyl acetate (3×) and the combined organics were washed with saturated sodium bicarbonate and brine, dried (MgSO4), and concentrated in vacuo to give 16C (0.98 g, 93%) as a beige solid. MS (ESI) m/z 225.1 (M+H)+.

1. temperatureThe reaction mixture was cooled to rt
2. filtrationfiltered
3. washwashed with ethyl acetate
4. additionSodium bicarbonate solution was added until it
5. extractionThe reaction mixture was extracted with ethyl acetate (3×)
6. washthe combined organics were washed with saturated sodium bicarbonate and brine
7. dry with materialdried (MgSO4)
8. concentrationconcentrated in vacuo