反应详情

温度

0 °C

Under argon, 142 mg (0.33 mmol) of the compound from example 1 were initially charged in THF (9.5 ml), the mixture was cooled to 0° C. and 0.33 ml (0.33 mmol) of sodium bis(trimethylsilyl)amide (1.0 M in THF) was then added dropwise. The mixture was stirred at 0° C. for 30 min, and 35 μl (0.43 mmol) of iodoethane were then added dropwise. The reaction mixture was stirred at RT overnight. The reaction mixture was diluted with ethyl acetate and washed twice with saturated aqueous sodium bicarbonate solution. The organic phase was dried over magnesium sulfate, filtered and concentrated. The residue was chromatographed on silica gel (mobile phase dichloromethane:methanol 60:1) and the product fractions were concentrated. This gave 89 mg (59% of theory) of the title compound as a solid.

1. stirringThe reaction mixture was stirred at RT overnight
2. washwashed twice with saturated aqueous sodium bicarbonate solution
3. dry with materialThe organic phase was dried over magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was chromatographed on silica gel (mobile phase dichloromethane:methanol 60:1)
7. concentrationthe product fractions were concentrated