反应详情

To a suspension of NaH (54.6 g, 60%, 1.365 mol) in 600 mL of DMF was added di-t-Butyl malonate (118 g, 0.546 mol) at 0° C. and stirred for 30 min. 2,4,6 trifluoronitrobenzene was added as a solution in 400 mL of DMF (75 g, 0.42 mol) over 3 hours and the solution stirred at ambient temperature for 12 hours. The reaction mixture was extracted with ethyl acetate (3×'s). The ethyl acetate was washed with water (3×'s) and with brine and dried over MgSO4 and concentrated to give 62 g of crude product. LCMS [M+Na]—396; 1H NMR (500 MHz, DMSO) δ 7.81 (m, 1H), 7.27 (m, 1H), 5.00 (s, 1H), 1.41 (m, 18H).

1. stirringthe solution stirred at ambient temperature for 12 hours
2. extractionThe reaction mixture was extracted with ethyl acetate (3×'s)
3. washThe ethyl acetate was washed with water (3×'s) and with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated