反应详情

1,3-Dibromopropane (8.5 mL, 82.0 mmol, 10 eq.) was added to a solution of compound 49 (2.0 g, 8.2 mmol) in DMF (20 mL). Then NaH (0.6 g, 15.0 mmol) was added in portions. The temperature rose to 50-60° C. The mixture was stirred at this temperature for 20 min (TLC monitoring, eluent: CH2Cl2). Then the mixture was carefully poured into ice. The product was extracted with ethyl acetate, and the extract was evaporated. The residue was washed from 1,3-dibromopropane with hexane. The resulting product was dissolved in CH2Cl2 and purified on a short thick column with silica gel, eluent: hexane-CH2Cl2 100:0→0:100. Compound 50 (1.87 g, 62%) was isolated as rapidly crystallizable oil.

1. customrose to 50-60° C
2. additionThen the mixture was carefully poured into ice
3. extractionThe product was extracted with ethyl acetate
4. customthe extract was evaporated
5. washThe residue was washed from 1,3-dibromopropane with hexane
6. dissolutionThe resulting product was dissolved in CH2Cl2
7. custompurified on a short thick column with silica gel, eluent