反应详情

温度

70 °C

To 1,3,4,5-tetrahydro-benzo[b]azepin-2-one (1 g, 6.2 mmol) in MeOH (8 mL), concentrated sulfuric acid (0.5 mL) was added and the mixture was stirred at room temperature for 2 hrs and at 70° C. for an additional hr. The solvent was removed and DCM and water were added. The organic layer was removed and the aqueous layer was basified with sat NaHCO3 and extracted with EtOAc (3×). The combined organic layers were washed with brine, dried (Na2SO4) and concentrated in vacuo to yield 4-(2-amino-phenyl)-butyric acid methyl ester (0.93 g). MS [M+H]+: 194.1; tR=1.49 min. (method 1)

1. customThe solvent was removed
2. additionDCM and water were added
3. customThe organic layer was removed
4. extractionextracted with EtOAc (3×)
5. washThe combined organic layers were washed with brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated in vacuo