反应详情

温度

80 °C

To the product from Example 90B (0.43 g, 1.50 mmol) as a solution in tetrahydrofuran (20 mL) was added potassium tert-butoxide (1.0 M in tetrahydrofuran) (1.80 mL, 1.80 mmol) via syringe under nitrogen followed by the addition of ethyl 2-bromoacetate (0.18 mL, 1.65 mmol). The reaction mixture heated at 80° C. and stirred overnight. The reaction mixture was cooled to room temperature, concentrated, diluted with ethyl acetate, washed with water and brine, dried with MgSO4, filtered and concentrated. Silica gel chromatography eluting with ethyl acetate/hexane (1:4) gave the title compound. MS (DCI) m/z 374 (M+H)+.

1. temperatureThe reaction mixture was cooled to room temperature
2. concentrationconcentrated
3. additiondiluted with ethyl acetate
4. washwashed with water and brine
5. dry with materialdried with MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. washSilica gel chromatography eluting with ethyl acetate/hexane (1:4)