反应详情

A solution of 2-(2,2-dimethyl-5-oxo-[1,3]dioxolan-4-ylidene)-N-(4-fluorobenzyl)-N-methoxy-acetamide (0.64 g, 2.07 mmol) in methanol (50 ml), was treated at 22° C. with 0.025 ml of a 4.6 M solution of sodium methoxide in methanol and the resulting mixture was stirred for 2 h at the same temperature. The reaction mixture was then quenched by the addition of 1 ml of 1 N hydrochloric acid and the solvent was concentrated under reduced pressure. The residue was diluted with ethyl acetate, washed with water and brine and then dried over anhydrous magnesium sulfate. Evaporation of the solvent and crystallization of the residue from a mixture of ethyl acetate and hexane gave 0.559 g (95% yield) of the title ester as white prisms; mp 71° C. 1HNMR 400 MHz (CDCl3) δ (ppm), mixture of rotamers, major: 3.69 (3H, s, OCH3), 3.89 (3H, s, OCH3), 4.80 (2H, s, NCH2), 6.45 (1H, s, CH), 7.03 (2H, m, aromatics), 7.30 (2H, m, aromatics). Anal. calcd for C13H14FNO5: C, 55.12; H, 4.98; N, 4.94. Found: C, 54.95; H, 4.73; N, 4.67.

1. customThe reaction mixture was then quenched by the addition of 1 ml of 1 N hydrochloric acid
2. concentrationthe solvent was concentrated under reduced pressure
3. additionThe residue was diluted with ethyl acetate
4. washwashed with water and brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customEvaporation of the solvent and crystallization of the residue
7. additionfrom a mixture of ethyl acetate and hexane