HRID1258935

反应详情

EQUATION

反应方程式

HRID 1258935 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirring solution of ethyl 3-(benzylamino)-4-nitrobenzoate (1.52 g, 5 mmol) in ethanol (50 mL) and acetic acid (7 mL) was added zinc dust (2.3 g, 35 mmol). After 1 hr at room temperature, the solids were filtered and the remaining solution was concentrated. The resulting residue was diluted with ethyl acetate (200 mL) and washed with dilute aq. NaHCO3 (1×100 mL), then the organic layer was dried (MgSO4), filtered and then concentrated to provide 1.44 g (˜100%) of crude ethyl 4-amino-3-(benzylamino)benzoate as an orange/brown oil. This material was used without further purification.

WORKUP

后处理

  1. filtrationthe solids were filtered
  2. concentrationthe remaining solution was concentrated
  3. additionThe resulting residue was diluted with ethyl acetate (200 mL)
  4. washwashed with dilute aq. NaHCO3 (1×100 mL)
  5. dry with materialthe organic layer was dried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated