RARECHEM AL BO 0005 1759-53-1 C4H6O2
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Production method
1. Take γ-butyrolactone as raw material, in the presence of halogenating agent and alcohol, open the ring to form γ-chlorobutyric acid butyl ester, in the presence of strong alkali, close the ring to obtain cyclopropanecarboxylic acid ester, and by hydrolysis to obtain cyclopropanecarboxylic acid.
2. Method: In a reaction flask equipped with a stirrer, thermometer, reflux condenser and dropping funnel, add 1400 mL of water and 160 g (4 mol) of sodium hydroxide, dissolve and cool to 0°C in an ice-salt bath. Add 240g (1.5mol) of bromine slowly and dropwise with stirring, keeping the reaction temperature below 10°C for about 20min. Cool to 0°C and slowly add cyclopropyl methyl ketone
(2) 42g (0.5mol), control the reaction solution not to exceed 10℃. Distill the reaction with water vapour to remove the bromomethane produced. After distillation and cooling, slowly add concentrated hydrochloric acid until the Congo red test paper is acidic. The solution is pale yellow and a small amount of sodium bisulphite solution is added. Saturate with sodium chloride and extract with ether. The ether layers are combined and dried over anhydrous sodium sulphate. The ether was evaporated and the fraction was fractionated under reduced pressure and collected at 92°C/2.926 kPa to give colourless cyclopropanecarboxylic acid
(1) 33 g, 76% yield.
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