CN104478751A - Preparation method of p-amino benzamide glutamic acid - Google Patents
Preparation method of p-amino benzamide glutamic acid Download PDFInfo
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- CN104478751A CN104478751A CN201410760835.7A CN201410760835A CN104478751A CN 104478751 A CN104478751 A CN 104478751A CN 201410760835 A CN201410760835 A CN 201410760835A CN 104478751 A CN104478751 A CN 104478751A
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- glutamic acid
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Abstract
The invention discloses a preparation method of p-amino benzamide glutamic acid. The preparation method comprises the following steps of (1) adding 180g/ml glutamic acid and a paranitrobenzoyl chloride condensate into a water solution, and stirring until the 180g/ml glutamic acid and the paranitrobenzoyl chloride condensate are sufficiently dissolved to prepare a p-amino benzamide glutamic acid water solution with the weight ratio of 35%; (2) regulating the pH value to 7.3, adding 52g/ml ammonium chloride, heating to 55 DEG C, adding 63g/ml gray cast iron powder, heating to 75 DEG C, pre-corroding for 2.5 hours, heating to 85 DEG C, and preserving the heat for 3.5 hours; and (3) filtering to remove iron mud, washing with distilled water, adding carbon for discoloring, crystallizing, carrying out suction filtration, washing, and drying to obtain a finished product of p-amino benzamide glutamic acid. By using the preparation method of p-amino benzamide glutamic acid, disclosed by the invention, the reaction conversion rate is increased, and the environment pollution is reduced.
Description
Technical field
The present invention relates to the preparation method of NSC 71042.
Background technology
At present, the preparation process of NSC 71042, reaction conversion ratio is low, and environmental pollution is more serious.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of NSC 71042, improve reaction conversion ratio, reduce environmental pollution.
For achieving the above object, technical scheme of the present invention designs a kind of preparation method of NSC 71042, comprises the steps:
1) L-glutamic acid of 180g/ml and paranitrobenzoyl chloride condenses drop in the aqueous solution, are stirred to abundant dissolving, are made into the aqueous solution that weight ratio is the p-nitrophenyl carbamylglutamic of 35%;
2) regulate pH value to be 7.3, drop into the ammonium chloride of 52g/ml, be warming up to 55 DEG C, add the graphitic cast iron powder of 63g/ml, be warming up to 75 DEG C, pre-erosion 2.5 hours, is warming up to 85 DEG C, is incubated 3.5 hours;
3) excessively filter iron mud, with aquae destillata washing, add carbon decoloring, crystallization, filtering and washing, dry to obtain NSC 71042 finished product.
Advantage of the present invention and beneficial effect are: the preparation method providing a kind of NSC 71042, improve reaction conversion ratio, reduce environmental pollution.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is further described.Following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
The technical scheme that the present invention specifically implements is:
A preparation method for NSC 71042, comprises the steps:
1) L-glutamic acid of 180g/ml and paranitrobenzoyl chloride condenses drop in the aqueous solution, are stirred to abundant dissolving, are made into the aqueous solution that weight ratio is the p-nitrophenyl carbamylglutamic of 35%;
2) regulate pH value to be 7.3, drop into the ammonium chloride of 52g/ml, be warming up to 55 DEG C, add the graphitic cast iron powder of 63g/ml, be warming up to 75 DEG C, pre-erosion 2.5 hours, is warming up to 85 DEG C, is incubated 3.5 hours;
3) excessively filter iron mud, with aquae destillata washing, add carbon decoloring, crystallization, filtering and washing, dry to obtain NSC 71042 finished product.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (1)
1. the preparation method of NSC 71042, is characterized in that, comprises the steps:
1) L-glutamic acid of 180g/ml and paranitrobenzoyl chloride condenses drop in the aqueous solution, are stirred to abundant dissolving, are made into the aqueous solution that weight ratio is the p-nitrophenyl carbamylglutamic of 35%;
2) regulate pH value to be 7.3, drop into the ammonium chloride of 52g/ml, be warming up to 55 DEG C, add the graphitic cast iron powder of 63g/ml, be warming up to 75 DEG C, pre-erosion 2.5 hours, is warming up to 85 DEG C, is incubated 3.5 hours;
3) excessively filter iron mud, with aquae destillata washing, add carbon decoloring, crystallization, filtering and washing, dry to obtain NSC 71042 finished product.
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CN201410760835.7A CN104478751A (en) | 2014-12-13 | 2014-12-13 | Preparation method of p-amino benzamide glutamic acid |
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CN201410760835.7A CN104478751A (en) | 2014-12-13 | 2014-12-13 | Preparation method of p-amino benzamide glutamic acid |
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CN104478751A true CN104478751A (en) | 2015-04-01 |
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CN201410760835.7A Pending CN104478751A (en) | 2014-12-13 | 2014-12-13 | Preparation method of p-amino benzamide glutamic acid |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105439895A (en) * | 2015-12-30 | 2016-03-30 | 浙江汇能生物股份有限公司 | Preparation method of N (4-aminobenzoyl)-L-glutamic acid |
CN110668968A (en) * | 2019-09-24 | 2020-01-10 | 涉县津东经贸有限责任公司 | Preparation method of p-aminobenzoyl glutamic acid |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101182323A (en) * | 2007-12-26 | 2008-05-21 | 潘福星 | Method for preparing folic acid |
-
2014
- 2014-12-13 CN CN201410760835.7A patent/CN104478751A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101182323A (en) * | 2007-12-26 | 2008-05-21 | 潘福星 | Method for preparing folic acid |
Non-Patent Citations (4)
Title |
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HAYRULLAH YILMAZ: "Resolution of (±)-β-Methylphenylethylamine by a Novel Chiral Stationary Phase for Pirkle-Type Column Chromatography", 《CHIRALITY》, vol. 22, 3 June 2009 (2009-06-03) * |
YANLIS: "N-(4-氨基苯甲酰)-L-谷氨酸", 《百度百科》, 6 August 2014 (2014-08-06) * |
袁杰 等: "催化加氢合成对氨基苯甲酰谷氨酸新工艺研究", 《精细化工中间体》, vol. 34, no. 4, 31 August 2004 (2004-08-31) * |
邵伟清: "N-对氨基苯甲酰-L-谷氨酸的制备", 《中国医药工业杂志》, vol. 35, no. 1, 31 December 2004 (2004-12-31) * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105439895A (en) * | 2015-12-30 | 2016-03-30 | 浙江汇能生物股份有限公司 | Preparation method of N (4-aminobenzoyl)-L-glutamic acid |
CN105439895B (en) * | 2015-12-30 | 2018-02-27 | 浙江汇能生物股份有限公司 | A kind of preparation method of N- p-benzoyls-Pidolidone |
CN110668968A (en) * | 2019-09-24 | 2020-01-10 | 涉县津东经贸有限责任公司 | Preparation method of p-aminobenzoyl glutamic acid |
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