反应详情

To a solution of 2-(chlorocarbonyl)phenyl acetate (20 mmol, 3.96 g) in toluene (50 ml) were N-ethyl-N,N-diisopropylamine (22 mmol, 2.84 g) and 2-methylalanine (22 mmol, 2.27 g) added. After stirring the reaction mixture at room temperature overnight, the mixture was diluted with 250 ml toluene and was washed with 1.8% HCl/aq (250 ml) and sat. NaCl/aq (250 ml). The organic phase was dried over Na2SO4 and concentrated under reduced pressure. The residue was dissolved in MeOH (50 mL) and 3 drops of conc. H2SO4 were added. The mixture was refluxed for 2 hours and concentrated under reduced pressure. The residue was dissolved in 250 mL EtOAc and washed with sat. NaHCO3/aq (250 ml) and sat. NaCl/aq (250 ml). The organic phase was dried over Na2SO4 and concentrated at reduced pressure. The resulting crude material was used without further purification.

1. additionadded
2. washwas washed with 1.8% HCl/aq (250 ml) and sat. NaCl/aq (250 ml)
3. dry with materialThe organic phase was dried over Na2SO4
4. concentrationconcentrated under reduced pressure
5. dissolutionThe residue was dissolved in MeOH (50 mL)
6. addition3 drops of conc. H2SO4 were added
7. temperatureThe mixture was refluxed for 2 hours
8. concentrationconcentrated under reduced pressure
9. dissolutionThe residue was dissolved in 250 mL EtOAc
10. washwashed with sat. NaHCO3/aq (250 ml) and sat. NaCl/aq (250 ml)
11. dry with materialThe organic phase was dried over Na2SO4
12. concentrationconcentrated at reduced pressure
13. customThe resulting crude material was used without further purification