反应详情

A mixture containing 4-(4-methyl-benzyl)-piperidin-4-ol (5.1 g, 25 mmol), 2-bromoethanol (1.8 ml, 25 mmol) and K2CO3 (5.2 g, 37.5 mmol) in 2-butanone (120 ml) was refluxed for 22 hours. H2O (30 ml) was added and the aqueous phase was extracted with ethylacetate. Combined organic phases were dried over Na2SO4, and concentrated. The residue was chromatographed over silica gel (CH2Cl2 --MeOH, 9:1 +NH4OH (1%)) to provide 1-(2-hydroxy-ethyl)-4-(4-methyl-benzyl)-piperidin-4-ol (4.3 g, 73%) as a yellow oil, MS: m/e=235.3 (M+).

1. temperaturewas refluxed for 22 hours
2. extractionthe aqueous phase was extracted with ethylacetate
3. dry with materialCombined organic phases were dried over Na2SO4
4. concentrationconcentrated
5. customThe residue was chromatographed over silica gel (CH2Cl2 --MeOH, 9:1 +NH4OH (1%))