反应详情

The title compound was prepared from dimethyloxalate (47.24 g, 400 mmol) and 4′-methylacetophenone (26.84 g, 200 mmol) using the procedure for Example 1d. Work-up and recrystallization provided the title compound as white needles (32.6 g, 74% yield). Mp 82–84° C. 1H NMR (300 MHz, CDCl3) δ 15.36 (br.s, 1H), 7.92 (d, J=8.3 Hz, 2H), 7.32 (d, J=8.3 Hz, 2H), 7.08 (s, 1H), 3.96 (s, 3H), 2.46 (s, 3H). Mass spectrum (API-TIS) m/z 221 (MH+). Anal calcd. for C12H12O4: C, 65.45; H, 5.49. Found: C, 65.46; H, 5.53.

1. customrecrystallization