Method for preparing ortho-chloromandelic acid
A technology of o-chloromandelic acid and sodium mandelate, which is applied in the field of organic synthesis, can solve the problems of increasing labor intensity and high price, and achieve the effects of reducing labor intensity, reducing production costs, and high purity
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Embodiment 1
[0026] In a 1000ml three-necked flask, add 100ml (0.887mol) of o-chlorobenzaldehyde, 160ml (1.87mol) of chloroform and 10g (0.044mol) of triethylbenzyl ammonium chloride (TEBA) powder, and heat up to 60°C. Slowly add 250ml of 50% sodium hydroxide solution prepared in advance dropwise under stirring at high temperature. After the dropwise addition, keep warm for 1 hour, add 500ml of water to dilute and cool the reaction solution to room temperature, and separate the lower layer of chloroform. Use 3mol / L hydrochloric acid solution to adjust the pH of the solution to 1, add 250ml of ethyl acetate for extraction, separate the water phase and ethyl acetate, and then extract the water phase twice with 120ml and 60ml of ethyl acetate respectively, combine the three extractions of ethyl acetate, and subtract Concentrate under reduced pressure to remove 400 ml of ethyl acetate to obtain crude o-chloromandelic acid in the form of yellow oil.
Embodiment 2
[0028] Add 40g of solid sodium hydroxide, 200ml of water, and 80ml of toluene to the yellow oily o-chloromandelic acid crude product remaining in Example 1, heat to 80°C, keep warm for 1 hour, cool, separate the water phase, and then use 3mol / L hydrochloric acid for the water phase Adjust the pH of the solution to 1, add 250ml of ethyl acetate for extraction, separate the water phase and ethyl acetate, and then extract the water phase with 120ml and 60ml of ethyl acetate, respectively, and combine three extractions of ethyl acetate. After the ethyl acetate was removed by evaporation under reduced pressure, 250ml of toluene was added, stirred and cooled to room temperature, and a little o-chloromandelic acid crystal was added as a seed crystal, the precipitated crystal was filtered by suction, and dried to obtain 91.5g of a white crystalline product. Yield 55.3%, mp: 87.0°C to 88.5°C.
Embodiment 3
[0030] In a 250ml three-necked flask, add 20ml (0.177mol) of o-chlorobenzaldehyde, 32ml (0.38mol) of chloroform and 2g (0.009mol) of triethylbenzyl ammonium chloride (TEBA), and raise the temperature to 60°C. Slowly add 50ml of 50% sodium hydroxide solution prepared in advance dropwise under stirring, and the rest is according to the method in Example 1 to obtain the crude product of yellow oily o-chloromandelic acid, add 250ml of toluene to the remaining yellow oil, and filter with suction to obtain Yellow sticky solid, after drying, 16.3g was obtained, mp<80°C, the solid was recrystallized with 30ml of toluene to obtain 14.5g of a yellowish refined product, the total yield in two steps was 43.9%, mp: 82.5°C-84.5°C.
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