HRID334722

反应详情

EQUATION

反应方程式

HRID 334722 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

2-Chloro-N-methyl-6-nitrobenzenamine (1.5 g, 8.0 mmol) was dissolved in a mixture of EtOH (15 mL) and H2O (15 ml). Iron powder (2.2 g, 40 mmol) was added followed by Acetic acid (0.55 mL, 9.6 mmol). The reaction was monitored by TLC, after 30 min, the reaction was completed. The reaction mixture was filtered over celite pad and the filtrate was neutralized by saturated NaHCO3 (10 mL). The product was extracted by EtOAc (2*10 mL), the organic layer was washed with brine (10 mL), dried over MgSO4 and concentrated to dryness to afford 920 mg of 6-chloro-N1-methylbenzene-1,2-diamine (Yield: 73%) as dark brown oil.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered over celite pad
  2. extractionThe product was extracted by EtOAc (2*10 mL)
  3. washthe organic layer was washed with brine (10 mL)
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated to dryness