HRID1156834

反应详情

EQUATION

反应方程式

HRID 1156834 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

30 g (0.155 mol) of 2,6-dimethyl-N-methoxyacetylaniline and 0.3 g of triethyl-benzyl-ammonium chloride were dissolved in a two-phase system mixture of 100 ml of 50% strength sodium hydroxide solution and 250 ml of toluene, and 19 g (0.016 mol) of propargyl bromide were added, whilst stirring vigorously. The mixture was stirred for 4 hours and the toluene phase was separated off, washed several times with water, dried over sodium sulphate and concentrated by distilling off the solvent under a waterpump vacuum. The residue was distilled under a high vacuum. 26.5 g (74% of theory) of 2,6-dimethyl-N-methoxyacetyl-N-propargyl-aniline of boiling point 140°/0.4 mm Hg and of melting point 49°-51° C. were obtained. ##STR178##

WORKUP

后处理

  1. additionwere added
  2. stirringThe mixture was stirred for 4 hours
  3. customthe toluene phase was separated off
  4. washwashed several times with water
  5. dry with materialdried over sodium sulphate
  6. concentrationconcentrated
  7. distillationby distilling off the solvent under a waterpump vacuum
  8. distillationThe residue was distilled under a high vacuum