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A kind of preparation technology of d-phenylglycine methyl ester hydrochloride crystallization

A technology of phenylglycine methyl ester and preparation process, which is applied in the preparation of organic compounds, cyanide reaction preparation, organic chemistry and other directions, can solve the problems of production difficulties, high production energy consumption, and insufficient utilization of reaction heat in downstream enterprises, and achieves The effect of low production cost, simple production process and excellent color grade

Active Publication Date: 2019-01-22
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method has the following main problems in the synthesis process: one, the first step reaction is an exothermic reaction, and the reaction temperature needs to be controlled by cooling; while the second step requires to be carried out at a higher temperature and needs to be heated, the whole synthesis process has no Make full use of the reaction heat, and the production energy consumption is high
Cause difficulties for the production of downstream enterprises

Method used

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  • A kind of preparation technology of d-phenylglycine methyl ester hydrochloride crystallization

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Experimental program
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Effect test

Embodiment 1

[0026] Weigh 70g of D-phenylglycine, measure 300mL of methanol, add them into a 500mL four-neck flask reactor in turn, start stirring, after mixing evenly, measure 60mL of thionyl chloride, and slowly dissolve thionyl chloride through a constant pressure dropping funnel Add it into the flask, drop it for 1.5 hours, keep the temperature in the reactor at 55°C during the dropwise addition, keep the temperature in the reactor at 60°C after the dropwise addition, reflux for 0.5h, and the reaction ends. Then control the temperature in the reactor at 45°C, stir the liquid in the reactor, add cyclohexane to the reactor for vacuum azeotropic distillation, maintain the vacuum degree in the reactor at 0.05MPa, and add the entrainer continuously Add to keep the liquid level in the reactor constant. After the mass content of methanol in the solution in the reactor is lower than 20%, stop the vacuum azeotropic distillation, carry out temperature-controlled cooling and crystallization, cont...

Embodiment 2

[0028] Weigh 25g of D-phenylglycine, measure 200mL of methanol, add them into a 500mL four-neck flask reactor in turn, start stirring, and after mixing evenly, measure 20mL of thionyl chloride, and dilute the thionyl chloride through a constant pressure dropping funnel. Slowly add to the reaction system, keep the temperature in the reactor at 50°C during the dropwise addition, control the temperature of the reactor at 65°C after the dropwise addition, reflux for 1 hour, and the reaction is completed. Then the temperature in the reactor is controlled at 40°C, the liquid in the reactor is stirred, and the entrainer toluene with 30% volume of the solution in the reactor is quickly added to the reactor to carry out vacuum azeotropic distillation, and the vacuum degree in the reactor is maintained at 0.08 MPa, when the volume of the distillate reaches the volume of toluene added, add the toluene of the same volume again, after adding 4 times, when the mass content of methanol in the...

Embodiment 3

[0030] Weigh 94g of D-phenylglycine, measure 300mL of methanol, add them into a 500mL four-neck flask reactor in turn, start stirring, after mixing evenly, measure 85mL of thionyl chloride, and slowly dissolve thionyl chloride through a constant pressure dropping funnel Add it into the reaction system, drop it for 1.5 hours, keep the temperature in the reactor at 50°C during the dropping process, and control the temperature of the reactor at 60°C to reflux for 1 hour after the dropwise addition, and the reaction is complete. Then control the temperature in the reactor at 40°C, stir the liquid in the reactor, add n-hexane to the reactor for vacuum azeotropic distillation, and add the entrainer continuously to keep the liquid level in the reactor constant . The vacuum degree in the reactor is maintained at 0.07MPa. When the mass content of methanol in the solution in the reactor is lower than 5%, the vacuum azeotropic distillation is stopped, and the temperature is controlled fo...

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Abstract

The invention belongs to the technical field of the chemical industry, and in particular relates to a preparation process of D-phenylglycine methyl ester hydrochloride crystals. The preparation process comprises the following steps: sequentially adding methanol and D-phenylglycine into a reactor, stirring uniformly, and slowly adding sulfoxide chloride; controlling the temperature in the reactor below 55DEG C, and controlling the temperature in the reactor to be 55-65DEG C after adding sulfoxide chloride; performing reflux reaction, then performing vacuum azeotropic distillation, and finally performing temperature controlled cooling crystallization; and filtering, washing and drying to obtain a D-phenylglycine methyl ester hydrochloride crystal product. The preparation process provided by the invention is high in one-pass yield, the prepared product is high in purity, good in color grade and stable in quality, the preparation process is low in production cost, and the operation is easy to control.

Description

technical field [0001] The invention belongs to the field of preparation of pharmaceutical intermediates, and in particular relates to a preparation process for crystallization of D-phenylglycine methyl ester hydrochloride. Background technique [0002] D-phenylglycine methyl ester hydrochloride, English name D-(-)-α-phenylglycine methyl esterhydrochloride (CAS No.: 19883411), molecular formula C 9 h 11 NO 2 .HCl, melting point 189-191°C, relative molecular mass 201.65, specific rotation ([α]20 / D): +120°(c=1, H 2 O), D-phenylglycine methyl ester hydrochloride is white powder or crystallization, if wherein mixed with impurity, product can be slightly yellow or gray, easy to absorb moisture. The structural formula is as follows: [0003] [0004] D-phenylglycine methyl ester is the active side chain of cefaclor and cephalexin synthesized by enzymatic method. Its molecular structure contains amino group, which is easy to oxidize and polymerize, has poor stability and is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C229/36C07C227/18
Inventor 孙华刘宝树任凯张军立王亚川崔雪君
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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