反应详情

温度

50 °C

To a mixture of (R)-1-methyl-piperidine-3-ol (4.61 g, 0.040 mol) and hydroxy-diphenyl-acetic acid methyl ester (9.63 g, 0.040 mol) in cyclohexane (50 ml) is added preactivated 4A molecular sieves and the mixture heated to 50° C. Sodium metal (50 mg) is then added and the resulting mixture heated to reflux. After 1 hour further sodium (50 mg) is added and reflux maintained for 5 hours. Concentration, re-dissolution in chloroform and washing with water followed by brine, drying over magnesium sulphate, filtration and evaporation gives a crude product. Purification by vacuum flash silica chromatography (gradient elution: DCM to DCM:methanol 20:1) gives, after evaporation, the title product as a foam.

1. additionis added
2. temperaturethe resulting mixture heated to reflux
3. temperaturereflux
4. temperaturemaintained for 5 hours
5. concentrationConcentration, re-dissolution in chloroform
6. washwashing with water
7. dry with materialdrying over magnesium sulphate, filtration and evaporation