反应详情

Bromoacetic acid ethyl ester (14.2 g, 9.37 ml, 84.8 mmol) was added dropwise to a soln. of cyclopropylamine (19.4 g; 23.5 ml, 0.34 mol) in EtOH (100 ml), while cooling with ice. The reaction mixture was stirred at RT for 18 h and then concentrated i. vac. Water was added to the residue and the mixture was extracted with CHCl3 (5×100 ml). The combined organic phases were washed with half-saturated sodium chloride soln., dried with Na2SO4 and concentrated i. vac. The crude product was distilled at approx. 85° C. under 24 mbar. Yield: 12.03 g (99%)

1. concentrationconcentrated i
2. additionWater was added to the residue
3. extractionthe mixture was extracted with CHCl3 (5×100 ml)
4. washThe combined organic phases were washed with half-saturated sodium chloride soln
5. dry with material, dried with Na2SO4
6. concentrationconcentrated i
7. distillationThe crude product was distilled at approx. 85° C. under 24 mbar