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General procedure: 2,3-Dihydrobenzo[b]-[1,4] dioxinecarboxylic acid A, B and C (10 mmol) in ethanol (200 mL) was treated with thionyl chloride (5 mL) under reflux overnight. Excess ethanol was distilled out and the solid left was dissolved in ethyl acetate (150 mL), washed with saturation sodium bicarbonate (200 mL) and then sodium chloride (200 mL). After drying the organic layer with anhydrous Na2SO4 and evaporating the solvent under reduced pressure and solid appeared. The solid was recrystallized from ethanol to obtain the compound A1, B1 and C1. The completion of the reaction was monitored on TLC by using silica gel-G coated plates by using ethyl acetate and petroleum ether (1 : 1) as the elution and observed in UV light.
With sulfuric acid; at 80℃; for 10h;
To 50 ml of ethanol was added 10 g of 1,4-benzodioxane-5-carboxylic acid, Slowly drip 3ml concentrated sulfuric acid, reflux at 80°C , the reaction 10h. After completion of the reaction, the solvent was evaporated, 20 ml of ethyl acetate was added, washed three times with saturated sodium chloride, dried over anhydrous sodium sulfate, Flash column chromatography to give colorless transparent oily liquid 1,4-benzodioxane-5-carboxylate.
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