反应详情

温度

40 °C

To a solution of 13-4 (2.23 g, 6.9 mmol) in 40 mL of THF was added triethylamine (2.2 mL), followed by the dropwise addition of methyliodide (0.43 mL, 6.9 mmol). The reaction mixture was heated to 40° C. for 2 h. The solvent was then removed in vacuo and the residue was taken up in EtOAc and washed two times with 100 mL portions of saturated aqueous ammonium chloride and a 100 mL portion of brine. The combined organic layers were dried over MgSO4 filtered and concentrated to dryness in vacuo. Then 150 mL of CH2Cl2 were added and the resulting precipitate was collected by vacuum filtration to give title compound 13-5.

1. customThe solvent was then removed in vacuo
2. washwashed two times with 100 mL portions of saturated aqueous ammonium chloride
3. dry with materialThe combined organic layers were dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated to dryness in vacuo
6. additionThen 150 mL of CH2Cl2 were added
7. filtrationthe resulting precipitate was collected by vacuum filtration