CN109467522B - 一种生产高纯度酚磺乙胺的方法 - Google Patents
一种生产高纯度酚磺乙胺的方法 Download PDFInfo
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- CN109467522B CN109467522B CN201811428838.5A CN201811428838A CN109467522B CN 109467522 B CN109467522 B CN 109467522B CN 201811428838 A CN201811428838 A CN 201811428838A CN 109467522 B CN109467522 B CN 109467522B
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- HBGOLJKPSFNJSD-UHFFFAOYSA-N Etamsylate Chemical compound CC[NH2+]CC.OC1=CC=C(O)C(S([O-])(=O)=O)=C1 HBGOLJKPSFNJSD-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229960004817 etamsylate Drugs 0.000 title claims abstract description 44
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000001816 cooling Methods 0.000 claims abstract description 27
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims abstract description 16
- IKQCSJBQLWJEPU-UHFFFAOYSA-N 2,5-dihydroxybenzenesulfonic acid Chemical compound OC1=CC=C(O)C(S(O)(=O)=O)=C1 IKQCSJBQLWJEPU-UHFFFAOYSA-N 0.000 claims abstract description 10
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- 238000010438 heat treatment Methods 0.000 claims description 17
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- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 9
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
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- 239000000498 cooling water Substances 0.000 claims description 5
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 3
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
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- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
- C07C303/06—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfuric acid or sulfur trioxide
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
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CN110642756A (zh) * | 2019-10-18 | 2020-01-03 | 海南顿斯医药科技有限公司 | 一种1/20水酚磺乙胺化合物 |
CN114380723A (zh) * | 2020-10-19 | 2022-04-22 | 成都益安成贸易有限公司 | 一种对羟基苯磺酸盐化合物及其制备方法和用途 |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
ES8104214A1 (es) * | 1980-05-24 | 1981-04-01 | Farmhispania | Procedimiento para la obtencion de derivados terapeuticos activos del acido 2,5-dihidroxi-bencen sulfonico |
ES2005425A6 (es) * | 1987-10-30 | 1989-03-01 | Induspol Sa | Procedimiento de preparacion de la sal de dietlamina del acido 2,5-dihidroxibencenosulfonico. |
WO2009083940A2 (en) * | 2008-01-03 | 2009-07-09 | Action Medicines S.L. | Processes for the preparation of 2,5-dihydroxybenzenesulfonic acid salts |
CN102920690A (zh) * | 2011-08-12 | 2013-02-13 | 王康俊 | 一种治疗脑心血管疾患的化学药 |
CN102942509A (zh) * | 2012-10-17 | 2013-02-27 | 山东方明药业集团股份有限公司 | 一种酚磺乙胺的合成方法 |
CN104447428A (zh) * | 2014-12-07 | 2015-03-25 | 河南领先科技药业有限公司 | 一种酚磺乙胺的制备方法 |
-
2018
- 2018-11-27 CN CN201811428838.5A patent/CN109467522B/zh active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
ES8104214A1 (es) * | 1980-05-24 | 1981-04-01 | Farmhispania | Procedimiento para la obtencion de derivados terapeuticos activos del acido 2,5-dihidroxi-bencen sulfonico |
ES2005425A6 (es) * | 1987-10-30 | 1989-03-01 | Induspol Sa | Procedimiento de preparacion de la sal de dietlamina del acido 2,5-dihidroxibencenosulfonico. |
WO2009083940A2 (en) * | 2008-01-03 | 2009-07-09 | Action Medicines S.L. | Processes for the preparation of 2,5-dihydroxybenzenesulfonic acid salts |
CN102920690A (zh) * | 2011-08-12 | 2013-02-13 | 王康俊 | 一种治疗脑心血管疾患的化学药 |
CN102942509A (zh) * | 2012-10-17 | 2013-02-27 | 山东方明药业集团股份有限公司 | 一种酚磺乙胺的合成方法 |
CN104447428A (zh) * | 2014-12-07 | 2015-03-25 | 河南领先科技药业有限公司 | 一种酚磺乙胺的制备方法 |
Non-Patent Citations (3)
Title |
---|
止血敏合成新工艺的研究;王晓丽等;《沈阳化工》;19961231(第2期);5-6页 * |
酚磺乙胺合成工艺改进;靳广毅和曾荣华;《现代应用药学》;19960831;第13卷(第4期);17页 * |
酚磺乙胺的合成工艺改进;赵海桥等;《药学研究》;20131231;第32卷(第2期);742页 * |
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