反应详情

温度

0 °C

To a solution of diphenylphosphite (2.25 mL) in dichloromethane at 0° C. was added t-butylbromoacetate (1.48 mL) followed by triethylamine (1.95 mL). The mixture was stirred at 0° C. for 15 min and then at rt for 1 h before being quenched with water and extracted into ethyl acetate, dried over MgSO4 and concentrated. The residue was purified by silica gel chromatography eluting with hexane/ethyl acetate to give the title compound. 1H NMR (500 MHz, CDCl3): δ 7.40-7.18 (m, 10H); 3.22 (s, 1H); 3.18 (s, 1H); 1.50 (s, 9H).

1. customat rt for 1 h before being quenched with water
2. extractionextracted into ethyl acetate
3. dry with materialdried over MgSO4
4. concentrationconcentrated
5. customThe residue was purified by silica gel chromatography
6. washeluting with hexane/ethyl acetate