反应详情

In 70 ml of a mixture of dimethylsulfoxide-tetrahydrofuran (1:1) are dissolved 12.3 g of trimethylene glycol and 15 g of tetradecyl bromide. To the solution is added 12 g of powdery potassium hydroxide. The mixture is vigorously stirred for one hour at a room temperature, which is refluxed under heating for two hours. The reaction mixture is poured into 400 ml of cold water, which is neutralized and subjected to extraction with ethyl acetate, then washed with water and dried. The resultant is concentrated to dryness, and the residue is dissolved in methanol when hot. Cooling of the solution gives precipitation of crystals, which are removed by filtration. The filtrate is refined by means of chromatography employing silica-gel (eluent:chloroform) to give 5.1 g of the end-product.

1. temperaturewhich is refluxed
2. temperatureunder heating for two hours
3. extractionsubjected to extraction with ethyl acetate
4. washwashed with water
5. customdried
6. concentrationThe resultant is concentrated to dryness
7. dissolutionthe residue is dissolved in methanol when hot
8. temperatureCooling of the solution
9. customgives
10. customprecipitation of crystals, which
11. customare removed by filtration