HRID1156833

反应详情

EQUATION

反应方程式

HRID 1156833 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

55 g (0.5 mol) of methoxyacetyl chloride were added dropwise to a solution of 61 g (0.5 mol) of 2,6-dimethylaniline and 50.5 g (0.5 mol) of triethylamine in 250 ml of toluene at 5° to 15° C., while stirring and cooling. The mixture was subsequently stirred at 20° C. for 2 hours, filtered and concentrated and the residue was taken up in water. The aqueous mixture was extracted with methylene chloride and the extract was dried over sodium sulphate and concentrated by distilling off the solvent. The residue was distilled under a high vacuum. 55 g (57% of theory) of 2,6-dimethyl-N-methoxyacetyl-aniline of boiling point 122°-132° C./0.1 mm Hg and of melting point 61°-63° C. were obtained. ##STR177##

WORKUP

后处理

  1. temperaturecooling
  2. stirringThe mixture was subsequently stirred at 20° C. for 2 hours
  3. filtrationfiltered
  4. concentrationconcentrated
  5. extractionThe aqueous mixture was extracted with methylene chloride
  6. dry with materialthe extract was dried over sodium sulphate
  7. concentrationconcentrated
  8. distillationby distilling off the solvent
  9. distillationThe residue was distilled under a high vacuum