HRID1293168

反应详情

EQUATION

反应方程式

HRID 1293168 的结构方程式

PROCEDURE

实验过程

Methyl 4-{(1S)-1-[(tert-butoxycarbonyl)amino]ethyl}benzoate (12.83 g, 45.9 mmol) was treated with trifluoroacetic acid (100 mL) and dichloromethane (100 mL) at room temperature for 16 h. After removal of the solvent, the residue was diluted with 10% hydrogen chloride solution in methanol (100 mL). The mixture was concentrated under reduced pressure and the residue was washed with ethyl acetate to give 9.40 g (95%) of the title compounds as white solids: 1H-NMR (DMSO-d6) δ 8.67 (2H, br.s), 8.01 (2H, d, J=8.4 Hz), 7.68 (2H, d, J=8.4 Hz), 4.49 (1H, q, J=6.9 Hz), 3.87 (3H, s), 1.53 (3H, d, J=6.9 Hz).

WORKUP

后处理

  1. customAfter removal of the solvent
  2. additionthe residue was diluted with 10% hydrogen chloride solution in methanol (100 mL)
  3. concentrationThe mixture was concentrated under reduced pressure
  4. washthe residue was washed with ethyl acetate