CN108752381A - A kind of preparation method of biphosphonate - Google Patents
A kind of preparation method of biphosphonate Download PDFInfo
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- CN108752381A CN108752381A CN201810774071.5A CN201810774071A CN108752381A CN 108752381 A CN108752381 A CN 108752381A CN 201810774071 A CN201810774071 A CN 201810774071A CN 108752381 A CN108752381 A CN 108752381A
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- added
- room temperature
- solution
- biphosphonate
- washed
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 60
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000243 solution Substances 0.000 claims abstract description 29
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000007864 aqueous solution Substances 0.000 claims abstract description 24
- 239000012074 organic phase Substances 0.000 claims abstract description 24
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 24
- FRPZMMHWLSIFAZ-UHFFFAOYSA-N 10-undecenoic acid Chemical compound OC(=O)CCCCCCCCC=C FRPZMMHWLSIFAZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- ASMQGLCHMVWBQR-UHFFFAOYSA-N Diphenyl phosphate Chemical class C=1C=CC=CC=1OP(=O)(O)OC1=CC=CC=C1 ASMQGLCHMVWBQR-UHFFFAOYSA-N 0.000 claims abstract description 12
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 12
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 12
- 239000011734 sodium Substances 0.000 claims abstract description 12
- 239000011780 sodium chloride Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/655—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having oxygen atoms, with or without sulfur, selenium, or tellurium atoms, as the only ring hetero atoms
- C07F9/65515—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having oxygen atoms, with or without sulfur, selenium, or tellurium atoms, as the only ring hetero atoms the oxygen atom being part of a five-membered ring
- C07F9/65517—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having oxygen atoms, with or without sulfur, selenium, or tellurium atoms, as the only ring hetero atoms the oxygen atom being part of a five-membered ring condensed with carbocyclic rings or carbocyclic ring systems
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
Abstract
A kind of preparation method of biphosphonate, including：Step 1:15.87g is added in 250mL there-necked flasks（0.050mol）And 0.050g;Step 2:The sodium hydroxide containing 4.00g is added（0.10mol）Aqueous solution 80mL, stir 0.5h at room temperature;Step 3:After uniform purple solution to be formed, 26.68g chlorinated diphenyl phosphates are added dropwise（0.10mol）Dichloromethane solution 100mL, control drop rate, 2h complete;Step 4:The sodium chloride of the undecenoic acid sodium and 0.2g of 0.1g is added, then proceedes to react at room temperature overnight until solution purple disappears;Step 5:After standing, organic phase is isolated;Step 6:Organic phase is washed about 3-5 times with 2% sodium hydrate aqueous solution;Step 7:Then it is washed with deionized 3-5 times.
Description
Technical field
The present invention relates to a kind of preparation methods of biphosphonate.
Background technology
The preparation method in the prior art for not finding suitable biphosphonate.
Invention content
A kind of preparation method of biphosphonate, including：
Step 1:15.87g is added in 250mL there-necked flasks（0.050mol）And 0.050g;
Step 2:The sodium hydroxide containing 4.00g is added（0.10mol）Aqueous solution 80mL, stir 0.5h at room temperature;
Step 3:After uniform purple solution to be formed, 26.68g chlorinated diphenyl phosphates are added dropwise（0.10mol）Dichloromethane
Solution 100mL, controls drop rate, and 2h is completed;
Step 4:The sodium chloride of the undecenoic acid sodium and 0.2g of 0.1g is added, then proceedes to react at room temperature overnight until solution
Purple disappears;
Step 5:After standing, organic phase is isolated;
Step 6:Organic phase is washed about 3-5 times with 2% sodium hydrate aqueous solution;
Step 7:Then it is washed with deionized 3-5 times;
Step 8:Finally revolving removes solvent and obtains being flaxen vitreous solid at room temperature
。
This biphosphonate of the present invention can be applied to field of biological pharmacy, chemical field, catalyst field.
Inventive point is：1）Complete reaction process；2）Material used；3）Concrete component.
Specific implementation mode
Embodiment 1
A kind of preparation method of biphosphonate, including：
Step 1:15.87g is added in 250mL there-necked flasks（0.050mol）And 0.050g;
Step 2:The sodium hydroxide containing 4.00g is added（0.10mol）Aqueous solution 80mL, stir 0.5h at room temperature;
Step 3:After uniform purple solution to be formed, 26.68g chlorinated diphenyl phosphates are added dropwise（0.10mol）Dichloromethane
Solution 100mL, controls drop rate, and 2h is completed;
Step 4:The sodium chloride of the undecenoic acid sodium and 0.2g of 0.1g is added, then proceedes to react at room temperature overnight until solution
Purple disappears;
Step 5:After standing, organic phase is isolated;
Step 6:Organic phase is washed about 3-5 times with 2% sodium hydrate aqueous solution;
Step 7:Then it is washed with deionized 3-5 times;
Step 8:Finally revolving removes solvent and obtains being flaxen vitreous solid at room temperature
。
This biphosphonate of the present invention can be applied to field of biological pharmacy, chemical field, catalyst field.
Embodiment 2
A kind of preparation method of biphosphonate, including：
Step 1:15.87g is added in 250mL there-necked flasks（0.050mol）And 0.050g;
Step 2:The sodium hydroxide containing 4.00g is added（0.10mol）Aqueous solution 80mL, stir 0.5h at room temperature;
Step 3:After uniform purple solution to be formed, 26.68g chlorinated diphenyl phosphates are added dropwise（0.10mol）Dichloromethane
Solution 100mL, controls drop rate, and 2h is completed;
Step 4:The sodium chloride of the undecenoic acid sodium and 0.2g of 0.12g is added, then proceedes to react at room temperature overnight until molten
Liquid purple disappears;
Step 5:After standing, organic phase is isolated;
Step 6:Organic phase is washed about 3-5 times with 2% sodium hydrate aqueous solution;
Step 7:Then it is washed with deionized 3-5 times;
Step 8:Finally revolving removes solvent and obtains being flaxen vitreous solid at room temperature
。
This biphosphonate of the present invention can be applied to field of biological pharmacy, chemical field, catalyst field.
Embodiment 4
A kind of preparation method of biphosphonate, including：
Step 1:15.87g is added in 250mL there-necked flasks（0.050mol）And 0.050g;
Step 2:The sodium hydroxide containing 4.00g is added（0.10mol）Aqueous solution 80mL, stir 0.5h at room temperature;
Step 3:After uniform purple solution to be formed, 26.68g chlorinated diphenyl phosphates are added dropwise（0.10mol）Dichloromethane
Solution 100mL, controls drop rate, and 2h is completed;
Step 4:The sodium chloride of the undecenoic acid sodium and 0.2g of 0.14g is added, then proceedes to react at room temperature overnight until molten
Liquid purple disappears;
Step 5:After standing, organic phase is isolated;
Step 6:Organic phase is washed about 3-5 times with 2% sodium hydrate aqueous solution;
Step 7:Then it is washed with deionized 3-5 times;
Step 8:Finally revolving removes solvent and obtains being flaxen vitreous solid at room temperature
。
This biphosphonate of the present invention can be applied to field of biological pharmacy, chemical field, catalyst field.
Embodiment 5
A kind of preparation method of biphosphonate, including：
Step 1:15.87g is added in 250mL there-necked flasks（0.050mol）And 0.050g;
Step 2:The sodium hydroxide containing 4.00g is added（0.10mol）Aqueous solution 80mL, stir 0.5h at room temperature;
Step 3:After uniform purple solution to be formed, 26.68g chlorinated diphenyl phosphates are added dropwise（0.10mol）Dichloromethane
Solution 100mL, controls drop rate, and 2h is completed;
Step 4:The sodium chloride of the undecenoic acid sodium and 0.2g of 0.15g is added, then proceedes to react at room temperature overnight until molten
Liquid purple disappears;
Step 5:After standing, organic phase is isolated;
Step 6:Organic phase is washed about 3-5 times with 2% sodium hydrate aqueous solution;
Step 7:Then it is washed with deionized 3-5 times;
Step 8:Finally revolving removes solvent and obtains being flaxen vitreous solid at room temperature
。
This biphosphonate of the present invention can be applied to field of biological pharmacy, chemical field, catalyst field.
Embodiment 6
A kind of preparation method of biphosphonate, including：
Step 1:15.87g is added in 250mL there-necked flasks（0.050mol）And 0.050g;
Step 2:The sodium hydroxide containing 4.00g is added（0.10mol）Aqueous solution 80mL, stir 0.5h at room temperature;
Step 3:After uniform purple solution to be formed, 26.68g chlorinated diphenyl phosphates are added dropwise（0.10mol）Dichloromethane
Solution 100mL, controls drop rate, and 2h is completed;
Step 4:The sodium chloride of the undecenoic acid sodium and 0.2g of 0.16g is added, then proceedes to react at room temperature overnight until molten
Liquid purple disappears;
Step 5:After standing, organic phase is isolated;
Step 6:Organic phase is washed about 3-5 times with 2% sodium hydrate aqueous solution;
Step 7:Then it is washed with deionized 3-5 times;
Step 8:Finally revolving removes solvent and obtains being flaxen vitreous solid at room temperature
。
This biphosphonate of the present invention can be applied to field of biological pharmacy, chemical field, catalyst field.
Embodiment 7
A kind of preparation method of biphosphonate, including：
Step 1:15.87g is added in 250mL there-necked flasks（0.050mol）And 0.050g;
Step 2:The sodium hydroxide containing 4.00g is added（0.10mol）Aqueous solution 80mL, stir 0.5h at room temperature;
Step 3:After uniform purple solution to be formed, 26.68g chlorinated diphenyl phosphates are added dropwise（0.10mol）Dichloromethane
Solution 100mL, controls drop rate, and 2h is completed;
Step 4:The sodium chloride of the undecenoic acid sodium and 0.2g of 0.17g is added, then proceedes to react at room temperature overnight until molten
Liquid purple disappears;
Step 5:After standing, organic phase is isolated;
Step 6:Organic phase is washed about 3-5 times with 2% sodium hydrate aqueous solution;
Step 7:Then it is washed with deionized 3-5 times;
Step 8:Finally revolving removes solvent and obtains being flaxen vitreous solid at room temperature
。
This biphosphonate of the present invention can be applied to field of biological pharmacy, chemical field, catalyst field.
Embodiment 8
A kind of preparation method of biphosphonate, including：
Step 1:15.87g is added in 250mL there-necked flasks（0.050mol）And 0.050g;
Step 2:The sodium hydroxide containing 4.00g is added（0.10mol）Aqueous solution 80mL, stir 0.5h at room temperature;
Step 3:After uniform purple solution to be formed, 26.68g chlorinated diphenyl phosphates are added dropwise（0.10mol）Dichloromethane
Solution 100mL, controls drop rate, and 2h is completed;
Step 4:The sodium chloride of the undecenoic acid sodium and 0.2g of 0.18g is added, then proceedes to react at room temperature overnight until molten
Liquid purple disappears;
Step 5:After standing, organic phase is isolated;
Step 6:Organic phase is washed about 3-5 times with 2% sodium hydrate aqueous solution;
Step 7:Then it is washed with deionized 3-5 times;
Step 8:Finally revolving removes solvent and obtains being flaxen vitreous solid at room temperature
。
This biphosphonate of the present invention can be applied to field of biological pharmacy, chemical field, catalyst field.
Embodiment 9
A kind of preparation method of biphosphonate, including：
Step 1:15.87g is added in 250mL there-necked flasks（0.050mol）And 0.050g;
Step 2:The sodium hydroxide containing 4.00g is added（0.10mol）Aqueous solution 80mL, stir 0.5h at room temperature;
Step 3:After uniform purple solution to be formed, 26.68g chlorinated diphenyl phosphates are added dropwise（0.10mol）Dichloromethane
Solution 100mL, controls drop rate, and 2h is completed;
Step 4:The sodium chloride of the undecenoic acid sodium and 0.2g of 0.19g is added, then proceedes to react at room temperature overnight until molten
Liquid purple disappears;
Step 5:After standing, organic phase is isolated;
Step 6:Organic phase is washed about 3-5 times with 2% sodium hydrate aqueous solution;
Step 7:Then it is washed with deionized 3-5 times;
Step 8:Finally revolving removes solvent and obtains being flaxen vitreous solid at room temperature
。
This biphosphonate of the present invention can be applied to field of biological pharmacy, chemical field, catalyst field.
Embodiment 10
A kind of preparation method of biphosphonate, including：
Step 1:15.87g is added in 250mL there-necked flasks（0.050mol）And 0.050g;
Step 2:The sodium hydroxide containing 4.00g is added（0.10mol）Aqueous solution 80mL, stir 0.5h at room temperature;
Step 3:After uniform purple solution to be formed, 26.68g chlorinated diphenyl phosphates are added dropwise（0.10mol）Dichloromethane
Solution 100mL, controls drop rate, and 2h is completed;
Step 4:The sodium chloride of the undecenoic acid sodium and 0.2g of 0.2g is added, then proceedes to react at room temperature overnight until solution
Purple disappears;
Step 5:After standing, organic phase is isolated;
Step 6:Organic phase is washed about 3-5 times with 2% sodium hydrate aqueous solution;
Step 7:Then it is washed with deionized 3-5 times;
Step 8:Finally revolving removes solvent and obtains being flaxen vitreous solid at room temperature
。
This biphosphonate of the present invention can be applied to field of biological pharmacy, chemical field, catalyst field.
Claims (2)
1. a kind of preparation method of biphosphonate, including：
Step 1:15.87g is added in 250mL there-necked flasks（0.050mol）And 0.050g;
Step 2:The sodium hydroxide containing 4.00g is added（0.10mol）Aqueous solution 80mL, stir 0.5h at room temperature;
Step 3:After uniform purple solution to be formed, 26.68g chlorinated diphenyl phosphates are added dropwise（0.10mol）Dichloromethane
Solution 100mL, controls drop rate, and 2h is completed;
Step 4:The sodium chloride of the undecenoic acid sodium and 0.2g of 0.1g is added, then proceedes to react at room temperature overnight until solution
Purple disappears;
Step 5:After standing, organic phase is isolated;
Step 6:Organic phase is washed about 3-5 times with 2% sodium hydrate aqueous solution;
Step 7:Then it is washed with deionized 3-5 times;
Step 8:Finally revolving removes solvent and obtains being flaxen vitreous solid at room temperature
。
2. this biphosphonate of the present invention can be applied to field of biological pharmacy, chemical field, catalyst field.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810774071.5A CN108752381A (en) | 2018-07-15 | 2018-07-15 | A kind of preparation method of biphosphonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810774071.5A CN108752381A (en) | 2018-07-15 | 2018-07-15 | A kind of preparation method of biphosphonate |
Publications (1)
| Publication Number | Publication Date |
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| CN108752381A true CN108752381A (en) | 2018-11-06 |
Family
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| CN201810774071.5A Withdrawn CN108752381A (en) | 2018-07-15 | 2018-07-15 | A kind of preparation method of biphosphonate |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257075A (en) * | 1998-12-14 | 2000-06-21 | 旭化成工业株式会社 | Method for preparing phosphate ester |
| CN1633441A (en) * | 2001-02-08 | 2005-06-29 | 阿克佐诺贝尔股份有限公司 | Process for purification of phosphate esters |
| CN101023067A (en) * | 2004-09-22 | 2007-08-22 | 茵迪斯佩克化学公司 | Phosphate ester flame retardants from resorcinol-ketone reaction products |
| CN101671439A (en) * | 2009-09-24 | 2010-03-17 | 浙江万盛化工有限公司 | Preparation method of macromolecular bisphenol A tetraphenyl diphosphate |
| WO2015030395A1 (en) * | 2013-08-30 | 2015-03-05 | 에스케이이노베이션 주식회사 | Novel oil marker and method for marking oil using same |
| CN108276439A (en) * | 2017-12-29 | 2018-07-13 | 湖州利鹏新材料科技有限公司 | A kind of brominated phosphate fire retardant and preparation method thereof |
-
2018
- 2018-07-15 CN CN201810774071.5A patent/CN108752381A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257075A (en) * | 1998-12-14 | 2000-06-21 | 旭化成工业株式会社 | Method for preparing phosphate ester |
| CN1633441A (en) * | 2001-02-08 | 2005-06-29 | 阿克佐诺贝尔股份有限公司 | Process for purification of phosphate esters |
| CN101023067A (en) * | 2004-09-22 | 2007-08-22 | 茵迪斯佩克化学公司 | Phosphate ester flame retardants from resorcinol-ketone reaction products |
| CN101671439A (en) * | 2009-09-24 | 2010-03-17 | 浙江万盛化工有限公司 | Preparation method of macromolecular bisphenol A tetraphenyl diphosphate |
| WO2015030395A1 (en) * | 2013-08-30 | 2015-03-05 | 에스케이이노베이션 주식회사 | Novel oil marker and method for marking oil using same |
| CN108276439A (en) * | 2017-12-29 | 2018-07-13 | 湖州利鹏新材料科技有限公司 | A kind of brominated phosphate fire retardant and preparation method thereof |
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Application publication date: 20181106 |