反应详情

温度

20 °C

HCl gas was bubbled through a solution of (S)-α-amino-4-methoxy-α-methyl-benzeneacetic acid, hydrochloride salt (2.0 g, 8.6 mmol) in EtOH (25 mL) at 4° C. The solution was stirred for 1 hour at 20° C. before being refluxed for 5 hours. After cooling, the solution was concentrated in vacuo. The resulting oil was dissolved in CH2Cl2, and washed with aq. NaHCO3 ; the aqueous phase was back-extracted with CH2Cl2. The combined organic fractions were washed with H2O, brine and dried over Na2SO4 prior to concentration to yield the title compound as a yellow oil (1.75 g, 91%).

1. temperaturebefore being refluxed for 5 hours
2. temperatureAfter cooling
3. concentrationthe solution was concentrated in vacuo
4. dissolutionThe resulting oil was dissolved in CH2Cl2
5. washwashed with aq. NaHCO3
6. extractionthe aqueous phase was back-extracted with CH2Cl2
7. washThe combined organic fractions were washed with H2O, brine
8. dry with materialdried over Na2SO4
9. concentrationto concentration