반응 #725879

반응 방정식

methyl salicylate

K2CO3

methyl chloroacetate

→

1

수율 17.0%

2-Methoxycarbonylmethoxy-benzoic acid methyl ester

수율 17.0%

용매

acetone

반응 조건

후처리

1. 1
   온도refluxed for 36 hours
2. 2
   workup.DISTILLATIONThe acetone was distilled off
3. 3
   workup.ADDITIONwater (1200 ml) was added
4. 4
   추출Crude 1 was extracted into chloroform
5. 5
   건조dried over Na2SO4
6. 6
   workup.DISTILLATIONdistilled
7. 7
   기타purified by column chromatography on silica gel

실험 절차

To a mixture of methyl salicylate (100 g, 657 mmol) and anhydrous K2CO3 (360 g, 2.605 mol) in anhydrous acetone (1000 ml) was added methyl chloroacetate (94 g, 866 mmol) and refluxed for 36 hours. The acetone was distilled off and water (1200 ml) was added. Crude 1 was extracted into chloroform, dried over Na2SO4 distilled and purified by column chromatography on silica gel using hexane as eluant to give pure 1 (25 grams, 17%) as a light yellow syrup.

출처