反应详情

温度

80 °C

A mixture of 2,8-diazaspiro[4.5]decan-1-one (3.03 g, 19.65 mmol), triethylamine (5.48 ml, 39.3 mmol) and ethyl 2-bromo-2-methylpropanoate (5.77 ml, 39.3 mmol) was heated at 80° C. overnight. The reaction mixture was partitioned between methylene chloride (200 mL) and saturated sodium bicarbonate, the alkaline phase was extracted with methylene chloride (3×100 mL). The combined organic phase was dried over magnesium sulfate, concentrated and the residue was purified on silica gel using methanol/methylene chloride to give the title compound. LC/MS (M+1)+: 269.4

1. customThe reaction mixture was partitioned between methylene chloride (200 mL) and saturated sodium bicarbonate
2. extractionthe alkaline phase was extracted with methylene chloride (3×100 mL)
3. dry with materialThe combined organic phase was dried over magnesium sulfate
4. concentrationconcentrated
5. customthe residue was purified on silica gel