HRID985460

反应详情

EQUATION

反应方程式

HRID 985460 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Chloro-1,3-dinitro-5-trifluoromethyl-benzene (5.43 g, 20.1 mmol) was dissolved in 10 mL anhydrous DMSO. Sodium methoxide (5.85 mL of a 25% w/w solution in methanol) was added by syringe. The yellow solution immediately turned pink-orange, with heat evolved. The reaction was left stirring overnight at room temperature, then EtOAc (300 mL) was added and the mixture was washed once with dilute HCl aqueous solution, thrice with water and once with brine. The organic solution was dried (Na2SO4), filtered and concentrated in vacuo. The residue was purified through a short plug of silica gel and 4.65 g of 2-methoxy-1,3-dinitro-5-trifluoromethylbenzene was isolated as a yellow solid.

WORKUP

后处理

  1. temperatureThe yellow solution immediately turned pink-orange, with heat
  2. waitThe reaction was left
  3. washthe mixture was washed once with dilute HCl aqueous solution, thrice with water and once with brine
  4. dry with materialThe organic solution was dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified through a short plug of silica gel