HRID2073387

反应详情

EQUATION

反应方程式

HRID 2073387 的结构方程式

PROCEDURE

实验过程

A mixture of 1,1,8-trimethyl-2-(1H)-naphtho[2,1-b]furanone (3.85)g, trifluoracetic acid (25 ml) and hexamine (3.5 g) was stirred under reflux for 18 h. The bulk of the trifluoroacetic acid was evaporated under reduced pressure and the residue was treated with water and heated at 90° for 10 minutes. The mixture was neutralised with potassium hydrogen carbonate and extracted twice with chloroform. The combined extracts were dried and evaporated to dryness, and the residue was recrystallised from ethyl acetate to give 7-formyl-1,1,8-trimethyl-2(1H)-naphtho[2,1-b]furanone (2.2 g), m.p. 193°-195° C.

WORKUP

后处理

  1. temperatureunder reflux for 18 h
  2. customThe bulk of the trifluoroacetic acid was evaporated under reduced pressure
  3. additionthe residue was treated with water
  4. temperatureheated at 90° for 10 minutes
  5. extractionextracted twice with chloroform
  6. customThe combined extracts were dried
  7. customevaporated to dryness
  8. customthe residue was recrystallised from ethyl acetate