preparation | 1-aminocyclopropyl methyl ester (3.41g,29.6mmol,1.0eq) is dissolved in 40ml of sulfuric acid aqueous solution a (1.62mL of 98% concentrated sulfuric acid is added to water to prepare, the molar equivalent of sulfuric acid is 1.0eq), the ice bath is cooled to 0-5 ℃, and 10ml of sodium nitrite (2.25g,32.6mmol,1.1eq) aqueous solution, stirring at room temperature for 1 hour. Then the above reaction droplets are added to the refluxed 100ml sulfuric acid aqueous solution B (obtained by adding 1.62mL 98% concentrated sulfuric acid into water, and the molar equivalent of sulfuric acid is 1.0eq). After dropping, stop heating and cool to room temperature. After TLC detection reaction is completed, ethyl acetate (3*100mL) is extracted three times, the organic phase is combined, dried with anhydrous magnesium sulfate, filtered and concentrated the organic phase to obtain methyl 1-hydroxy -1-cycloprocarboxylate (2.57g,22.1mmol), colorless oily liquid, and the yield is 74.8%. |