CN114965738B - 一种2,4-二氨基-6-羟基嘧啶起始物料纯度的hplc-uv检测方法 - Google Patents
一种2,4-二氨基-6-羟基嘧啶起始物料纯度的hplc-uv检测方法 Download PDFInfo
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- CN114965738B CN114965738B CN202210397234.9A CN202210397234A CN114965738B CN 114965738 B CN114965738 B CN 114965738B CN 202210397234 A CN202210397234 A CN 202210397234A CN 114965738 B CN114965738 B CN 114965738B
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- Prior art keywords
- diamino
- hydroxypyrimidine
- methanol
- purity
- sample solution
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- SWELIMKTDYHAOY-UHFFFAOYSA-N 2,4-diamino-6-hydroxypyrimidine Chemical compound NC1=CC(=O)N=C(N)N1 SWELIMKTDYHAOY-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000007858 starting material Substances 0.000 title claims abstract description 13
- 238000000825 ultraviolet detection Methods 0.000 title claims abstract description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 78
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229960000789 guanidine hydrochloride Drugs 0.000 claims abstract description 21
- PJJJBBJSCAKJQF-UHFFFAOYSA-N guanidinium chloride Chemical compound [Cl-].NC(N)=[NH2+] PJJJBBJSCAKJQF-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 20
- 239000012488 sample solution Substances 0.000 claims abstract description 14
- 238000010828 elution Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims abstract description 5
- 235000019796 monopotassium phosphate Nutrition 0.000 claims abstract description 5
- 239000012535 impurity Substances 0.000 claims description 19
- 238000001514 detection method Methods 0.000 claims description 13
- 239000012071 phase Substances 0.000 claims description 10
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 3
- 239000012074 organic phase Substances 0.000 claims description 2
- 239000013557 residual solvent Substances 0.000 claims description 2
- 238000011010 flushing procedure Methods 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 abstract description 2
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 11
- 239000003085 diluting agent Substances 0.000 description 7
- QJIUMVUZDYPQRT-UHFFFAOYSA-N 6-chloro-2,4-pyrimidinediamine Chemical compound NC1=CC(Cl)=NC(N)=N1 QJIUMVUZDYPQRT-UHFFFAOYSA-N 0.000 description 6
- 239000000523 sample Substances 0.000 description 5
- 239000008346 aqueous phase Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000010408 sweeping Methods 0.000 description 2
- ZFMITUMMTDLWHR-UHFFFAOYSA-N Minoxidil Chemical compound NC1=[N+]([O-])C(N)=CC(N2CCCCC2)=N1 ZFMITUMMTDLWHR-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229940125782 compound 2 Drugs 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229960003632 minoxidil Drugs 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
- G01N30/6052—Construction of the column body
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/55—Design of synthesis routes, e.g. reducing the use of auxiliary or protecting groups
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
Claims (1)
Priority Applications (1)
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CN202210397234.9A CN114965738B (zh) | 2022-04-15 | 2022-04-15 | 一种2,4-二氨基-6-羟基嘧啶起始物料纯度的hplc-uv检测方法 |
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CN202210397234.9A CN114965738B (zh) | 2022-04-15 | 2022-04-15 | 一种2,4-二氨基-6-羟基嘧啶起始物料纯度的hplc-uv检测方法 |
Publications (2)
Publication Number | Publication Date |
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CN114965738A CN114965738A (zh) | 2022-08-30 |
CN114965738B true CN114965738B (zh) | 2024-03-29 |
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CN202210397234.9A Active CN114965738B (zh) | 2022-04-15 | 2022-04-15 | 一种2,4-二氨基-6-羟基嘧啶起始物料纯度的hplc-uv检测方法 |
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
AU488952B2 (en) * | 1976-07-15 | 1976-09-30 | The Wellcome Foundation Limited | 2. 4-diamino-5-benzylpyrimidines |
HU900036D0 (en) * | 1989-01-04 | 1990-03-28 | Lonza Ag | Process for preparation of 2,4-diamino-6-pyperidinyl-pyrimidin-3-n-oxide |
EP1728872A1 (en) * | 2005-06-02 | 2006-12-06 | DSM IP Assets B.V. | Biosynthetic production of (5S,6S)-6-amino-5-hydroxycyclohexa-1,3-diene-1-carboxylic acid (2,3-CHA) |
CN112986432A (zh) * | 2021-02-20 | 2021-06-18 | 天科(荆州)制药有限公司 | 一种2,4-二氨基-6-氯嘧啶有关物质的检测方法及其应用 |
CN113754592A (zh) * | 2021-10-26 | 2021-12-07 | 江苏睿实生物科技有限公司 | 一种2,4-二胺基-6-氯嘧啶的制备方法 |
-
2022
- 2022-04-15 CN CN202210397234.9A patent/CN114965738B/zh active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
AU488952B2 (en) * | 1976-07-15 | 1976-09-30 | The Wellcome Foundation Limited | 2. 4-diamino-5-benzylpyrimidines |
HU900036D0 (en) * | 1989-01-04 | 1990-03-28 | Lonza Ag | Process for preparation of 2,4-diamino-6-pyperidinyl-pyrimidin-3-n-oxide |
US4959475A (en) * | 1989-01-04 | 1990-09-25 | Lonza Ltd. | Process for the production of 2,4-diamino-6-piperidinyl-pyrimidine-3-N-oxide |
EP1728872A1 (en) * | 2005-06-02 | 2006-12-06 | DSM IP Assets B.V. | Biosynthetic production of (5S,6S)-6-amino-5-hydroxycyclohexa-1,3-diene-1-carboxylic acid (2,3-CHA) |
CN112986432A (zh) * | 2021-02-20 | 2021-06-18 | 天科(荆州)制药有限公司 | 一种2,4-二氨基-6-氯嘧啶有关物质的检测方法及其应用 |
CN113754592A (zh) * | 2021-10-26 | 2021-12-07 | 江苏睿实生物科技有限公司 | 一种2,4-二胺基-6-氯嘧啶的制备方法 |
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Inventor after: Mei Qing Inventor after: Hu Jin Inventor after: Guan Danyingzi Inventor after: Yang Tao Inventor after: Chai Jinzhu Inventor before: Chai Jinzhu Inventor before: Mei Qing Inventor before: Hu Jin Inventor before: Guan Danyingzi Inventor before: Yang Tao |
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