反应详情

温度

115 °C

A mixture of 1-phenyl-hexane-1,4-dione (5 g), ethanol amine (1.6 g) and pivalic acid (2.15 g) in a solvent mixture containing n-heptane:tetrahydrofuran:toluene (4:1:1, 50 mL) was refluxed with stirring at 110-120° C. Water formed during the reaction was removed azeotropically during 3 to 4 hrs. The reaction mixture was cooled and the solvent was removed. The residue obtained was dissolved in dichloromethane (50 mL), washed with saturated sodium bicarbonate solution (50 mL), water (50 mL), and then with brine (50 mL), dried (Na2SO4) and the solvent was evaporated. The crude compound obtained as an oily mass. The crude substance was used in the next step without purification.

1. temperaturewas refluxed
2. customwas removed azeotropically during 3 to 4 hrs
3. temperatureThe reaction mixture was cooled
4. customthe solvent was removed
5. customThe residue obtained
6. washwashed with saturated sodium bicarbonate solution (50 mL), water (50 mL)
7. dry with materialwith brine (50 mL), dried (Na2SO4)
8. customthe solvent was evaporated