HRID1399685

反应详情

EQUATION

反应方程式

HRID 1399685 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-methoxy-4-methyl-1-nitrobenzene (5 g; 29.9 mmol) in methanol (200 mL) was added Tin(II) chloride dihydrate (33.7 g; 150 mmol) and the mixture was heated to reflux for 3 h. The solvent was removed under reduced pressure and the residue was dissolved in ethyl acetate. A saturated solution of sodium hydrogen carbonate was added until pH 8. A suspension formed and the mixture was filtered on a plug of celite. The organic phase was separated, washed with a saturated solution of sodium hydrogen carbonate solution and dried over magnesium sulphate. The solvent was removed under reduced pressure and the residue was used as such in the next reaction.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 3 h
  3. customThe solvent was removed under reduced pressure
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. additionA saturated solution of sodium hydrogen carbonate was added until pH 8
  6. customA suspension formed
  7. filtrationthe mixture was filtered on a plug of celite
  8. customThe organic phase was separated
  9. washwashed with a saturated solution of sodium hydrogen carbonate solution
  10. dry with materialdried over magnesium sulphate
  11. customThe solvent was removed under reduced pressure
  12. customsuch in the next reaction