反应详情

A mixture of 2.76 g salicylic acid, 2.02 g triethylamine and 3.5 gm 1-chloroethyl ethyl carbonate in 25 ml of toluene is refluxed for three hours. The reaction mixture is cooled and 25 ml of ether and 25 ml of water added. The organic layer is separated, washed 2× with 25 ml water, dried through sodium sulfate and concentrated in vacuo. The residue (3.88 g) is chromatographed on 200 g silica gel. Elution with 25% methylene chloride in hexane gives 1-(ethoxycarbonyloxy)ethyl salicylate which is directly used in the next step.

1. temperatureis refluxed for three hours
2. temperatureThe reaction mixture is cooled
3. customThe organic layer is separated
4. washwashed 2× with 25 ml water
5. dry with materialdried through sodium sulfate
6. concentrationconcentrated in vacuo
7. customThe residue (3.88 g) is chromatographed on 200 g silica gel
8. washElution with 25% methylene chloride in hexane