反应详情

To a solution of (1-Oxo-indan-2-yl)-acetic acid (Step 1, 2.00 g) in methanol (10 mL) at 0° C. was added sulphuric acid (2 mL). The solution was stirred for 2 h and then diluted with water (50 mL) and extracted with ethyl acetate. The combined organic layers were washed with sat. sodium hydrogenocarbonate, dried and concentrated to give (1-Oxo-indan-2-yl)-acetic acid methyl ester (pale yellow oil, 2.15 g, quantitative). C12H12O3; MW: 204.23; LCMS (method A) RT 1.40 min; ES 227 (25%, MNa+), 205 (25%, MH+), 173 (100%); IR: 2952, 1734, 1710, 1608, 1436 cm−1; 1H NMR (400 MHz, CDCl3) 7.78 (1H, d), 7.61 (1H, t), 7.47 (1H, d), 7.39 (1H, t), 3.70 (3H, s), 3.47 (1H, dd), 2.95-3.08 (2H, m), 2.89 (1H, dd), 2.63 (1H, dt) ppm. The compound was used without further purification for the next step

1. extractionextracted with ethyl acetate
2. washThe combined organic layers were washed with sat. sodium hydrogenocarbonate
3. customdried
4. concentrationconcentrated