HRID529643

反应详情

EQUATION

反应方程式

HRID 529643 的结构方程式

PROCEDURE

实验过程

To a solution of 4-amino-3-methoxybenzoic acid (1 equiv) in N—N-dimethylformamide (0.6 M) was added sodium bicarbonate (9.7 equiv), HATU (2 equiv) and methyl amine hydrochloride (10 equiv). The reaction mixture was stirred at room temperature overnight. The reaction mixture was poured on water and extracted with ethyl acetate. The organic layer was dried over sodium sulfate and concentrated under reduced pressure. The crude product was purified by column chromatography (silica gel 100-200 mesh, 0-10% methanol in DCM as eluent) to give the title compound. (Yield: 63%). MS (ESI) m/z 181 [M+1]+.

WORKUP

后处理

  1. additionThe reaction mixture was poured on water
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe crude product was purified by column chromatography (silica gel 100-200 mesh, 0-10% methanol in DCM as eluent)