反应详情

A pale yellow suspension of morpholine-3,5-dione (1.2 g, 10 mmol), of 1,3-dibromopropane (3.4 ml, 33 mmol), and potassium carbonate (2.7 g, 19 mmol) in 23 ml of 2-butanone is refluxed under an argon atmosphere for 22 hours. After cooling, the suspension is concentrated on a rotary evaporator, poured into ice/water, and extracted twice with ethyl acetate. The combined organic phases are washed with brine, dried over anhydrous sodium sulphate, and evaporated. The residual yellow oil (2.06 g) is purified by chromatography (Biotage 40 Mi, I=15 cm, cyclohexane/ethyl acetate 3:1).

1. temperatureAfter cooling
2. concentrationthe suspension is concentrated on a rotary evaporator
3. additionpoured into ice/water
4. extractionextracted twice with ethyl acetate
5. washThe combined organic phases are washed with brine
6. dry with materialdried over anhydrous sodium sulphate
7. customevaporated
8. customThe residual yellow oil (2.06 g) is purified by chromatography (Biotage 40 Mi, I=15 cm, cyclohexane/ethyl acetate 3:1)