反应详情

A solution of 1-bromomethyl-1-cyclohexene (3.25 g) and 2-aminoethanol (6 mL) in trichloroethylene (40 mL) was heated at the reflux temp. for 3 d, cooled to room temp., and diluted with a 1N NaOH solution (30 mL). The aqueous layer was extracted with CH2Cl2 (4×20 mL) and the combined organic layers were washed with H2O (30 mL) and a saturated NaCl solution (30 mL), dried (Na2SO4) and concentrated under reduced pressure. The residue was purified by vacuum distillation to give N-hydroxyethyl-N-cyclohex-1-enylmethylamine as a colorless oil (1.78 g, 62%): bp 92-94° C. (6 mmHg),

1. temperaturecooled to room temp.
2. extractionThe aqueous layer was extracted with CH2Cl2 (4×20 mL)
3. washthe combined organic layers were washed with H2O (30 mL)
4. dry with materiala saturated NaCl solution (30 mL), dried (Na2SO4)
5. concentrationconcentrated under reduced pressure
6. distillationThe residue was purified by vacuum distillation