HRID523229

反应详情

EQUATION

反应方程式

HRID 523229 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of N-(3-bromo-2-methylphenyl)-3,5-difluoro-2-nitrobenzamide (821 mg, 2.21 mmol), NH4Cl (1.18 g, 22.1 mmol) and zinc (1.45 g, 22.1 mmol) in MeOH (10 mL) was stirred at room temperature for 60 min. The mixture was filtered and the filtrate was concentrated. The residue was suspended in DCM and washed with saturated aqueous NaHCO3. The organic phase, with an insoluble precipitate, was separated from the aqueous phase and concentrated to give 2-amino-N-(3-bromo-2-methylphenyl) -3,5-difluorobenzamide (760 mg), used without further purification. Mass spectrum m/z 341, 343 (M+H)+, 363, 365 (M+Na)+.

WORKUP

后处理

  1. filtrationThe mixture was filtered
  2. concentrationthe filtrate was concentrated
  3. washwashed with saturated aqueous NaHCO3
  4. customThe organic phase, with an insoluble precipitate, was separated from the aqueous phase
  5. concentrationconcentrated