HRID1846302

反应详情

EQUATION

反应方程式

HRID 1846302 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 6-methoxy-1H-benzo[d][1,3]oxazine-2,4-dione (0.800 g, 4.10 mmol) and 4-bromoaniline (0.750 g, 4.30 mmol) in anhydrous DMF (10 mL) was stirred at 115° C. for 16 hours under nitrogen. DMF was removed and the residue was mixed with water (100 mL) and ethyl acetate (150 mL). The organic phase was separated, backwashed with brine (50 mL), and concentrated. The residue was purified by column chromatography (SiO2, hexane/ethyl acetate=1:1) to give 2-amino-N-(4-bromo-phenyl)-5-methoxy-benzamide. Yield: 0.240 g (18%).

WORKUP

后处理

  1. customDMF was removed
  2. additionthe residue was mixed with water (100 mL) and ethyl acetate (150 mL)
  3. customThe organic phase was separated
  4. concentrationconcentrated
  5. customThe residue was purified by column chromatography (SiO2, hexane/ethyl acetate=1:1)