Synthesis method of high-purity D-2-chloropropionyl chloride
A D-2-, chloropropionyl chloride technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylates, etc., can solve the problem that D-2-chloropropionyl chloride is not high in purity and is not suitable for chemical plant economy. Recycling, products and by-products are not easy to separate and other problems, to achieve the effect of improving the reaction yield and purity, low equipment requirements, and easy handling
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Embodiment 1
[0020] Step a, synthetic D-2-methyl chloropropionate
[0021] Add 110g of L-lactate methyl ester and 1.5g of pyridine to the dry reaction flask with stirring and condensation, cool down to -7°C in an ice-salt bath, add 140g of thionyl chloride dropwise, control the system temperature below 0°C, and add dropwise for 2 hours After completion, the ice-salt bath was pulled down and vacuum stirred for 1 hour, then the temperature was raised to 80°C, and refluxed for 4 hours. After the reaction solution dropped to 35°C, the SOCl gas was removed under reduced pressure. 2 , SO 2 Wait for the gas, after the gas is basically pumped out, add 30g of tap water and wash for 10min to obtain 128g of methyl chloropropionate with a yield of 99.2% and a purity of 99.6%.
[0022] Step b, synthesis of D-2-chloropropionic acid
[0023] Add 120g of methyl chloropropionate to the reaction flask with stirring, add 228g of 20% sodium hydroxide solution dropwise at a temperature below 10°C, finish add...
Embodiment 2
[0027] Step a, synthetic D-2-methyl chloropropionate
[0028] Add 150g of L-lactate methyl ester and 1.5g of pyridine to the dry reaction flask with stirring and condensation, cool down to -2°C in an ice-salt bath, add 190g of thionyl chloride dropwise, control the system temperature below 0°C, and add dropwise for 3 hours After completion, the ice-salt bath was pulled down and vacuum stirred for 2 hours, and then the temperature was raised to 60°C, and refluxed for 5 hours. After the reaction solution dropped to 35°C, the gases such as SOCl2 and SO2 were removed under reduced pressure. 174.6 g of methyl chloropropionate was obtained, with a yield of 99.2% and a purity of 99.4%.
[0029] Step b, synthesis of D-2-chloropropionic acid
[0030] Add 135g of methyl chloropropionate to a reaction flask with stirring, add 400g of 20% sodium hydroxide solution dropwise at a temperature below 5°C, and finish adding dropwise in 2 hours, keep warm at a temperature below 5°C for 3 hours,...
Embodiment 3
[0034] Step a, synthetic D-2-methyl chloropropionate
[0035] Add 150g of L-lactate methyl ester and 1.5g of pyridine to the dry reaction flask with stirring and condensation, cool down to -10°C in an ice-salt bath, add 190g of thionyl chloride dropwise, control the system temperature below 0°C, and add dropwise for 3 hours After completion, the ice-salt bath was pulled down and vacuum stirred for 2 hours, and then the temperature was raised to 55°C, and refluxed for 5 hours. After the reaction solution dropped to 35°C, the gases such as SOCl2 and SO2 were removed under reduced pressure. 174.6 g of methyl chloropropionate was obtained, with a yield of 99.2% and a purity of 99.4%.
[0036] Step b, synthesis of D-2-chloropropionic acid
[0037] Add 135g of methyl chloropropionate to the reaction flask with stirring, add 270g of sodium hydroxide solution with a mass fraction of 20% below 5°C dropwise, after 2 hours to complete the dropwise addition, keep warm at below 5°C for 3 ...
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