HRID2073387
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
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
- temperatureunder reflux for 18 h
- customThe bulk of the trifluoroacetic acid was evaporated under reduced pressure
- additionthe residue was treated with water
- temperatureheated at 90° for 10 minutes
- extractionextracted twice with chloroform
- customThe combined extracts were dried
- customevaporated to dryness
- customthe residue was recrystallised from ethyl acetate