反应详情

温度

110 °C

A mixture of the crude material from Example 2C (2.7 g, 8.5 mmol) in acetic acid (60 mL) and heated to 110° C. Then Zn (18 equivalents) was added slowly in potions over 30 min to the mixture under nitrogen. After the completion the mixture was cooled to room temperature and the Zn residue was filtered off. The filter cake was washed with MeOH. And the combined filtrate was stripped to dryness. The residue was dissolved in 70 mL of chloroform and washed with water twice. The chloroform solution was dried with anhydrous MgSO4 and concentrated to dryness. The crude product was purified by column chromatography (silica gel, 10% EtOAc/Hexane). Purified yield for the three steps from example 2B-2D was 1.11 g (43.3%).

1. temperatureAfter the completion the mixture was cooled to room temperature
2. filtrationthe Zn residue was filtered off
3. washThe filter cake was washed with MeOH
4. dissolutionThe residue was dissolved in 70 mL of chloroform
5. washwashed with water twice
6. dry with materialThe chloroform solution was dried with anhydrous MgSO4
7. concentrationconcentrated to dryness
8. customThe crude product was purified by column chromatography (silica gel, 10% EtOAc/Hexane)
9. customPurified
10. customyield for the three steps from example 2B-2D