反应详情

温度

100 °C

To the product of Step C of Example 129 (1.50 g, 4.40 mmol) was added POCl3 (5 mL, 53.6 mmol). The mixture was heated to 100° C. for 17 hours before concentrating in vacuo. The residue was dissolved in ethyl acetate and washed with NaHCO3 (saturated, aq.), water, dried (Na2SO4) and concentrated. The residue was purified by flash chromatography (silica gel) eluting with 10% ethyl acetate/hexane affording product. MS (electrospray) m/e 360.9 MH+ (Rt=4.1 min LC/MS).

1. concentrationbefore concentrating in vacuo
2. dissolutionThe residue was dissolved in ethyl acetate
3. washwashed with NaHCO3 (saturated, aq.), water
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated
6. customThe residue was purified by flash chromatography (silica gel)
7. washeluting with 10% ethyl acetate/hexane affording product