反应详情

温度

70 °C

To a stirred solution of the product from Step C, Example 1 (0.12 g, 0.32 mmol) in DMF (10 mL) was added potassium carbonate (0.15 g, 1.05 mmol) followed by benzyl 2-bromoacetate (0.08 g, 0.48 mmol) at room temperature and the mixture was heated at 70° C. for 20 h. A saturated aqueous solution of ammonium chloride (20 mL) was added followed by ethyl acetate (50 mL). The organic layer was separated and the aqueous was extracted with ethyl acetate (3×50 mL). The combined organic layers were washed with brine (30 mL), dried and evaporated to a residue, which was purified by chromatography (silica, 50% ethyl acetate in hexane) to give a solid (0.11 g, 71%): mp 140-141° C.; MS (ES) m/z 484 (M+).

1. customThe organic layer was separated
2. extractionthe aqueous was extracted with ethyl acetate (3×50 mL)
3. washThe combined organic layers were washed with brine (30 mL)
4. customdried
5. customevaporated to a residue, which
6. customwas purified by chromatography (silica, 50% ethyl acetate in hexane)