HRID1514889

反应详情

EQUATION

反应方程式

HRID 1514889 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 4-amino-3-nitro-benzoic acid (546 mg). EDCI (576 mg) and HOBt (405 mg) in DMF (8 mL) was added 3,4-dimethylaniline (363 mg) and the mixture was stirred at room temperature for 3 h. The mixture was poured into water and exreacted with EtOAc. The organic phase was washed with water (2×) and was dried over sodium sulfate. The solvent was concentrated to approximately 10 mL and the resulting precipitate was filtered, washed with EtOAc and dried under reduced pressure to give 4-amino-N-(3,4-dimethyl-phenyl)-3-nitro-benzamide as a yellow solid, mp=192-195° C.; MS (m/z) 284 (M−1).

WORKUP

后处理

  1. washThe organic phase was washed with water (2×)
  2. dry with materialwas dried over sodium sulfate
  3. concentrationThe solvent was concentrated to approximately 10 mL
  4. filtrationthe resulting precipitate was filtered
  5. washwashed with EtOAc
  6. customdried under reduced pressure