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Synthesizing method of L-2-sodium chloropropionate

The technology of a sodium chloropropionate and a synthesis method is applied in chemical instruments and methods, carboxylate preparation, carboxylate preparation and other directions, and can solve the problems of long distillation recovery time, low production efficiency, time-consuming and energy-consuming, etc., To achieve the effect of shortening the reaction time, improving efficiency and protecting the environment

Inactive Publication Date: 2016-07-06
福建仁宏医药化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because of the low boiling point of dichloromethane, two-stage condensation is used when distilling dichloromethane. The first stage is cooled with cold water, and the second stage is cooled with ice brine to ensure the recovery rate of dichloromethane; also because the extraction agent dichloromethane The consumption of dichloromethane is large, and the time of distillation recovery is very long, so the process of the whole distillation recovery of methylene chloride is time-consuming and energy-consuming, and the production efficiency is very low

Method used

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Examples

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preparation example Construction

[0023] A kind of synthetic method of L-2-sodium chloropropionate of the present invention comprises the steps:

[0024] 1) Preparation of L-2-chloropropionic acid

[0025] Concentration is 20%~40% hydrochloric acid (the impact of hydrochloric acid concentration on the reaction is shown in Table 1) is directly sucked or pumped in the reactor, and drop into solid L-2-alanine, stir and dissolve, when solid After dissolving, the temperature is cooled to below 0° by an ice bath (the impact of the reaction temperature on the reaction is as shown in Table 2), and the prepared sodium nitrite is added in portions under continuous stirring. Preferably, the concentration of sodium nitrite is 10% to 20%, the molar ratio of L-2-alanine to sodium nitrite is 1:1.8, the reaction of L-2-alanine and sodium nitrite in this range of molar ratio is relatively thorough, without affecting the normal When the reaction rate is low, the use of raw materials is saved, and the production cost is reduced...

Embodiment 1

[0037] 1) Preparation of L-2-chloropropionic acid

[0038] Draw or pump hydrochloric acid with a concentration of 20% directly into the reaction kettle, and put in solid L-2-alanine for stirring and dissolving. Add the prepared sodium nitrite in portions, preferably, the concentration of sodium nitrite is 10%, the molar ratio of L-2-alanine to sodium nitrite is 1:1.8, the L -2-alanine and sodium nitrite react relatively thoroughly, without affecting the normal reaction rate, save the use of raw materials, reduce production costs, dropwise at a speed of 5 seconds / drop, and within 3.5 hours After the internal dropwise addition, continue to stir at 0° for 3 to 4 hours, stop stirring after the reaction is over, let it stand for 2 to 3 hours, and then carry out suction filtration. Use a glass rod to transfer the above solution into the funnel, keep the height when the solution is added lower than the 2 / 3 position of the funnel, and put the oblique opening at the bottom of the funn...

Embodiment 2

[0044] 1) Preparation of L-2-chloropropionic acid

[0045] Draw or pump hydrochloric acid with a concentration of 28% directly into the reaction kettle, and put in solid L-2-alanine, stir and dissolve, when the solid dissolves, cool the temperature to below 0° in an ice bath, and continue stirring Add the prepared sodium nitrite in portions, preferably, the concentration of sodium nitrite is 10%, the molar ratio of L-2-alanine to sodium nitrite is 1:1.8, the L -2-alanine and sodium nitrite react relatively thoroughly, without affecting the normal reaction rate, save the use of raw materials, reduce production costs, dropwise at a speed of 5 seconds / drop, and within 3.5 hours After the internal dropwise addition, continue to stir at 0° for 3 to 4 hours, stop stirring after the reaction is over, let it stand for 2 to 3 hours, and then carry out suction filtration. Use a glass rod to transfer the above solution into the funnel, keep the height when the solution is added lower th...

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Abstract

The invention discloses a synthesizing method of L-2-sodium chloropropionate.The synthesizing method comprises the steps that hydrochloric acid is directly sucked or pumped into a reaction kettle, and L-2-aminopropionic acid solids are put into the reaction kettle; the temperature is lowered to 0 DEG C or below through an ice bath, prepared sodium nitrite is added in batches, stirring is stopped after reacting is finished, and standing under heat preservation is performed for 2-3 hours; suction filtration is performed, L-2-chloropropionic acid filtrate obtained through suction filtration is contained in a separating funnel oscillator to be extracted, obtained extracting solutions are merged after layering under standing is performed, alkali liquid is added into the merged extracting solution for a neutralization reaction, layering under standing is performed, an obtained oil layer is dichloromethane solvent, and a water layer is an aqueous solution of L-2-sodium chloropropionate.According to the synthesizing method of L-2-sodium chloropropionate, the alkali liquid is directly added into the dichloromethane extracting solution of L-2-chloropropionic acid for neutralization, distilling is replaced with layering, the whole dichloromethane distilling and recycling process is omitted, and therefore not only is the efficiency greatly improved, but also energy consumption is greatly reduced.

Description

technical field [0001] The present invention relates to a kind of synthetic method of sodium L-2-chloropropionate. Background technique [0002] Sodium L-2-chloropropionate is an essential intermediate for the synthesis of R-(+)-2-(4-hydroxyphenoxy)propionic acid, and R-(+)-2-(4-hydroxyphenoxy) Propionic acid is the most important raw material for the synthesis of phenoxypropionic acid herbicides. Sodium L-2-chloropropionate comes from the reaction of L-2-chloropropionic acid and lye, so to prepare sodium L-2-chloropropionate, L-2-chloropropionic acid must be prepared first. Usually, L-2-alanine is used as the starting material, and L-2-chloropropionic acid is prepared through steps such as diazotization, chlorination, extraction, and distillation. [0003] Pump or pump the measured hydrochloric acid directly into the reaction kettle, put in solid L-2-alanine, cool to below 0°, add sodium nitrite in stages, keep warm for several hours after adding, and filter with suction....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C53/19
CPCC07C51/412
Inventor 严招春
Owner 福建仁宏医药化工有限公司
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