HRID1649365

反应详情

EQUATION

反应方程式

HRID 1649365 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

15.9 g (0.1 mol) of 2,6-dimethyl-N-propargylaniline and 8 g (0.1 mol) of pyridine were heated to the boil in 100 ml of tetrahydrofuran, and 13 g (0.1 mol) of furan-2-carboxylic acid chloride were added carefully. The reaction mixture was stirred under reflux for 15 minutes and then concentrated by distilling off the solvent in vacuo. The residue was taken up in methylene chloride and the methylene chloride mixture was washed with water. The organic phase was separated off, dried over sodium sulphate and concentrated. After triturating with petroleum ether, the residue crystallized. 22.5 g (89% of theory) of 2,6-dimethyl-N-(2-furoyl)-N-propargyl-aniline of melting point 109°-112° C. were obtained.

WORKUP

后处理

  1. temperatureunder reflux for 15 minutes
  2. concentrationconcentrated
  3. distillationby distilling off the solvent in vacuo
  4. washthe methylene chloride mixture was washed with water
  5. customThe organic phase was separated off
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated
  8. customAfter triturating with petroleum ether
  9. customthe residue crystallized