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A p-hydroxyphenylglycine technology, which is applied in the preparation of organic compounds, organic chemistry, chemical instruments and methods, etc., can solve the problems of complicated process operation, increased cost, HPG color and purity that cannot meet the requirements of separation, etc.
Inactive Publication Date: 2009-02-11
谢建中
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However, the color and purity of HPG synthesized by this process cannot meet the requirements of separation, and must be refined to reach the standard, which not only increases the cost, but also makes the process operation complicated.
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example 1
[0022] Example 1: In a 5000L enamel reaction kettle, put 740Kg of 40% glyoxylic acid, 580Kg of water, 400Kg of molten phenol, 500Kg of sulfamic acid, and 5Kg of p-toluenesulfonic acid, stir and heat up to 70°C, keep the temperature for 12 hours, and the reaction is complete. Add 500Kg of water, 20Kg of sodium bisulfite, cool down to 45°C, add ammonia water dropwise, adjust the pH value to 4.2 within 2 hours, cool down to 40°C, centrifuge, wash with water until there is no foam, wash with methanol until the filtrate is colorless, and dry HPG374Kg was obtained, the content was 98.8%, and the yield was 56.0%.
example 2
[0023] Example 2: Put 740Kg of 40% glyoxylic acid, 580Kg of water, 400Kg of molten phenol, 500Kg of sulfamic acid, and 5Kg of p-toluenesulfonic acid into a 5000L enamel reaction kettle, stir and heat up to 35°C, and keep warm at 35-40°C for 6 hour, then be warming up to 65-70 ℃ of heat preservation reaction for 8 hours, other subsequent procedures are the same as example 1, obtain DL-HPG434Kg, content 98.9%, yield 65%.
example 3
[0024] Example 3: Except that the glyoxylic acid input was self-made 19.3% 1534Kg, other procedures were the same as Example 2 to obtain DL-HPG435Kg with a content (HPLC) of 98.8% and a yield of 65%.
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Abstract
The invention belongs to the field of pharmaceutical chemical engineering intermediate production, which relates to a synthesis technology of p-hydroxyphenylglycine (HPG). The purpose of the invention is achieved by the following steps: phenol, glyoxylic acid, water and sulfamic acid carry out the one-pot braise reaction under the action of catalysts such as benzene sulfonic acid, p-toluenesulfonic acid, o-toluenesulfonic acid, and the like; after the reaction is finished, a small amount of reducing substances such as sodium sulfite, sodium bisulfite, hydroxylamine hydrochloride, and the like, are added; finally, the PH value is adjusted by alkali, the mother liquor separation is washed by large amount of water and then washed by organic solvents such as methanol, ethanol, acetone, glacial acetic acid, and the like; the obtained product HPG is white powder, wherein, the content of NPLC is equal to or more than 98.5, which can meet the requirement of splitting. The method has the advantages of low production cost, simple operation, stable quality, etc.
Description
[0001] Field [0002] The technical field described in the present invention is the production field of pharmaceutical and chemical intermediates, and is about the preparation technology of compounds with the following structure: [0003] [0004] The chemical name is p-hydroxyphenylglycine (HPG for short), which is a racemic mixture obtained through chemical synthesis, and L-p-hydroxyphenylglycine is obtained after resolution, which is the side chain of semi-synthesized amoxicillin and cefadroxil. Background technique [0005] The classic synthesis method is to use p-hydroxybenzaldehyde and sodium cyanide to react through streck, ammonolysis, and hydrolysis to obtain the target product HPG. However, this method uses highly toxic sodium cyanide and has been eliminated. [0006] Phenol and glyoxylic acid can be condensed to produce p-hydroxymandelic acid, which can be converted into the target product HPG by ammonolysis, but p-hydroxymandelic acid is not easy to separate in ...
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