HRID1649363

反应详情

EQUATION

反应方程式

HRID 1649363 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

50 g (0.2 mol) of 2,6-dimethyl-N-(2-furoyl)-N-propargyl-aniline were dissolved in 200 ml of anhydrous tetrahydrofuran, and 150 mg of potassium tert.-butylate were added. During this procedure, the temperature of the solution rose to about 50° C., the solution becoming colored. The reaction mixture was left to stand for 2 hours and then poured onto 500 ml of water. The crystalline product which had precipitated was filtered off, dried and recrystallized from ethyl acetate/petroleum ether. 24 g (48% of theory) of 2,6-dimethyl-N-allenyl-N-(2-furoyl)-aniline of melting point 138°-41° C. were obtained. (The 1H-NMR spectrum indicated complete isomerization). ##STR99##

WORKUP

后处理

  1. customrose to about 50° C.
  2. waitThe reaction mixture was left
  3. customThe crystalline product which had precipitated
  4. filtrationwas filtered off
  5. customdried
  6. customrecrystallized from ethyl acetate/petroleum ether