HRID1465803

反应详情

EQUATION

反应方程式

HRID 1465803 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
62.5 °C

PROCEDURE

实验过程

To a solution of methyl 4-amino-2-methoxybenzoate (501 mg, 2.77 mmol) in ethanol (8 ml) was added acetic anhydride (0.42 ml, 4.44 mmol, 1.6 eq) and the clear solution heated at 60-65° C. for 2 h. After cooling to room temperature the solvent was removed by rotary evaporator and the residue treated with water (10 ml) and saturated sodium bicarbonate solution (10 ml) before extracting with ethyl acetate (20 ml, 2×10 ml). The combined ethyl acetate extract was washed with water, then brine, dried (MgSO4) and evaporated to give methyl 4-acetamido-2-methoxybenzoate (545 mg, 88%) as a white solid.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature the solvent
  2. customwas removed by rotary evaporator
  3. additionthe residue treated with water (10 ml) and saturated sodium bicarbonate solution (10 ml)
  4. extractionbefore extracting with ethyl acetate (20 ml, 2×10 ml)
  5. extractionThe combined ethyl acetate extract
  6. washwas washed with water
  7. dry with materialbrine, dried (MgSO4)
  8. customevaporated