反应详情

温度

150 °C

To a solution of α,α′-Bisbromo-m-xylene (10.02 g, 37.95 mmol) in DMF (20 mL) was added triethyl phosphite (3.15 g, 3.3 mL, 19.98 mmol) via syringe. The mixture was heated to 150° C. for 2 minutes in a microwave. The reaction mixture was poured into water and product extracted with diethyl ether (3×25 mL). The combined organics were washed with water (2×50 mL) and brine (50 mL), and dried over Na2SO4. Reduced volume in vacuo and purified product by flash column eluting 30-100% ethyl acetate in hexanes to give 4.64 g (76%) 60 as a colorless oil. LCMS: m/z for C12H18BrO3P++H observed 321.0 and 323.0 at 2.29 minutes of a 3.5 minute run, gradient 5-95% CH3CN in H2O.

1. extractionextracted with diethyl ether (3×25 mL)
2. washThe combined organics were washed with water (2×50 mL) and brine (50 mL)
3. dry with materialdried over Na2SO4
4. custompurified product by flash column
5. washeluting 30-100% ethyl acetate in hexanes