反应详情

To a solution of 2.4 g (10.3 mmol) of product from Step A in 50 ml DMF was added 6 g (44.8 mmol) lithium iodide. The resulting solution was refluxed under N2 for 2 hours. The reaction mixture was poured into 500 ml H2O/HCl and extracted with ethyl acetate. THe organic solution was washed with water; saturated NaCl, dried over MgSO4 and concentrated in vacuo to give 1.7 g crude product which was chromatographed through a pressure column eluting with 10% ethyl acetate/n-hexane to give 0.9 g of title compound.

1. temperatureThe resulting solution was refluxed under N2 for 2 hours
2. extractionextracted with ethyl acetate
3. washTHe organic solution was washed with water
4. dry with materialsaturated NaCl, dried over MgSO4
5. concentrationconcentrated in vacuo
6. customto give 1.7 g crude product which
7. customwas chromatographed through a pressure column
8. washeluting with 10% ethyl acetate/n-hexane