反应详情

温度

75 °C

To a solution of the Product from Example 1I (0.137 g, 0.36 mmol) in a mixture of water (0.75 mL), methanol (1.5 mL) and tetrahydrofuran (1.5 mL) was added iron (0.102 g, 1.82 mmol) and ammonium chloride (0.030 g, 0.54 mmol) and the resulting mixture was heated with vigorous stirred at 75° C. for one hour. The warm reaction mixture was filtered through celite and rinsed well with methanol and tetrahydrofuran. The filtrate was concentrated and partitioned between 10% NaHCO3 solution and ethyl acetate. The organic layer was dried over sodium sulfate, filtered, and concentrated to give a waxy solid that was used without purification (97%).

1. temperaturethe resulting mixture was heated
2. customThe warm reaction mixture
3. filtrationwas filtered through celite
4. washrinsed well with methanol and tetrahydrofuran
5. concentrationThe filtrate was concentrated
6. custompartitioned between 10% NaHCO3 solution and ethyl acetate
7. dry with materialThe organic layer was dried over sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated
10. customto give a waxy solid that
11. customwas used without purification (97%)