CN102328962A - Preparation method of tetramine platinum chloride - Google Patents
Preparation method of tetramine platinum chloride Download PDFInfo
- Publication number
- CN102328962A CN102328962A CN201110223209A CN201110223209A CN102328962A CN 102328962 A CN102328962 A CN 102328962A CN 201110223209 A CN201110223209 A CN 201110223209A CN 201110223209 A CN201110223209 A CN 201110223209A CN 102328962 A CN102328962 A CN 102328962A
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- CN
- China
- Prior art keywords
- preparation
- chlorination
- ammonia platinum
- platinum chloride
- platinum
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 title abstract 4
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 title abstract 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 22
- 150000003839 salts Chemical class 0.000 claims abstract description 15
- 239000007787 solid Substances 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- XKUTVNLXHINPAP-UHFFFAOYSA-N azane platinum Chemical compound N.[Pt] XKUTVNLXHINPAP-UHFFFAOYSA-N 0.000 claims description 23
- 238000005660 chlorination reaction Methods 0.000 claims description 23
- 238000004821 distillation Methods 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 abstract description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract description 5
- 239000006227 byproduct Substances 0.000 abstract description 4
- 238000010992 reflux Methods 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 abstract 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 125000004122 cyclic group Chemical group 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 10
- 238000009835 boiling Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000006837 decompression Effects 0.000 description 3
- 238000002330 electrospray ionisation mass spectrometry Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 190014017285 Satraplatin Chemical compound 0.000 description 1
- -1 amine platinum complexes Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000000118 anti-neoplastic effect Effects 0.000 description 1
- 125000003963 dichloro group Chemical group Cl* 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- FVIZARNDLVOMSU-UHFFFAOYSA-N ginsenoside K Natural products C1CC(C2(CCC3C(C)(C)C(O)CCC3(C)C2CC2O)C)(C)C2C1C(C)(CCC=C(C)C)OC1OC(CO)C(O)C(O)C1O FVIZARNDLVOMSU-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000003057 platinum Chemical class 0.000 description 1
- HRGDZIGMBDGFTC-UHFFFAOYSA-N platinum(2+) Chemical compound [Pt+2] HRGDZIGMBDGFTC-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229960005399 satraplatin Drugs 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a preparation method of a platinum complex, namely tetramine platinum chloride, which belongs to the field of pharmacochemistry. The preparation method comprises the following steps: carrying out a reaction on a Magnus salt and concentrated ammonia solution under the condition of heating reflux till the green Magnus salt disappears completely so as go generate pale yellow or colorless clear liquid, and concentrating to get a solid of the tetramine platinum chloride. According to the preparation method of the tetramine platinum chloride, the higher conversation rate is kept, the cyclic utilization of byproducts can be simultaneously achieved when a target compound is synthesized, the cost is saved, and the preparation method is suitable for large-batch industrial production and conductive to environmental protection.
Description
Technical field
The present invention relates to a kind of preparation of platinum complex chlorination four ammonia platinum, belong to the pharmaceutical chemistry field.
Background technology
Mixing amine platinum is a new direction of current platinum series antineoplastic medicament development, and its representative Satraplatin and ZD0473 have got into III clinical trial phase conceptual phase, platinic compound K [Pt (NH
3) Cl
3] be the important intermediate that preparation mixes amine platinum complexes, chlorination four ammonia platinum then are synthetic K [Pt (NH
3) Cl
3] one of principal reaction thing.Chlorination four ammonia platinum, full name dichloro four ammino platinum (II) [Tetraamminoplatinate (II) diChloride], molecular weight is 352.14, chemical structural formula:
Traditional chlorination four ammonia platinum preparing methods are the ammoniation process of cis-platinum, be about to cis-platinum with strong aqua under 40 ~ 50 ℃ of conditions, react chlorination four ammonia platinum, reaction process is:
The characteristics of this method are that transformation efficiency is high, can reach more than 95%, and shortcoming is to be reactant with the cis-platinum, causes cost to increase, and is not suitable for suitability for industrialized production.
Summary of the invention:
The object of the present invention is to provide a kind of productive rate high, cost is low, is fit to the chlorination four ammonia platinum preparing methods of suitability for industrialized production.
Technical scheme of the present invention is: with solid Magnus salt and strong aqua (24 ~ 28%) mixed by solid-to-liquid ratio: 1:3～4; Under normal pressure and boiling condition; Back flow reaction 6～8 hours all disappears until green Magnus salt, obtains faint yellow or colourless chlorination four ammonia platinum solution; By the ordinary method underpressure distillation, obtain faint yellow or colourless chlorination four ammonia platinum solids again.
Said solid Magnus salinity minor is [Pt (NH
3)
4] [PtCl
4], its structural formula is:
Magnus is synthetic K [Pt (NH
3) Cl
3] main by product in the process, purity is greater than 95%.
Said strong aqua is technical grade, and is commercially available, and concentration is 24 ~ 28%; The strong aqua add-on is 3～4 times of popular response ratio, adopts the method that refluxes simultaneously, can when realize higher conversion, reach ammoniacal liquor and utilize to greatest extent, prevents its volatilization, polluted air.
Simultaneous interpretation controlling Preparation Method of the present invention is compared, and following advantage is arranged:
Because the raw material that the preparation method adopted of chlorination four ammonia platinum of the present invention is a Magnus salt, and this material is synthetic K [Pt (NH
3) Cl
3] main by product in the engineering; Therefore compare with traditional cis-platinum ammoniation process; Chlorination four ammonia platinum preparing methods of the present invention are when having kept higher conversion, and cost has been practiced thrift in the recycle of by product when having reached synthesising target compound; Be applicable to large batch of suitability for industrialized production, help environment protection simultaneously.
Figure of description
Accompanying drawing 1 is chemical reaction flow process figure of the present invention.
Embodiment:
Below in conjunction with accompanying drawing and embodiment the present invention is done further elaboration, but content of the present invention is not limited to said scope.
Embodiment 1: take by weighing purity and be 96% 10gMagnus salt, join in the round-bottomed flask, add concentration and be 24% 30ml ammoniacal liquor; Under normal pressure, boiling condition; Backflow 8h, extremely green Magnus salt all disappears, and gets flaxen chlorination four ammonia platinum solution; With this solution decompression distillation, obtain faint yellow to colourless chlorination four ammonia platinum solid 3.49g.
Adopting model is 353 [M+H]
+EFI mass spectrograph (ESI-MS) carry out ultimate analysis: actual value N%15.97, H%3.50 Pt%55.48; Theoretical value N%15.91, H%3.41 Pt%55.40.
Embodiment 2: take by weighing purity and be 98% 20gMagnus salt, join in the round-bottomed flask, add concentration and be 26% 70ml ammoniacal liquor; Under normal pressure, boiling condition; Backflow 7h, extremely green Magnus salt all disappears, and gets faint yellow to colourless chlorination four ammonia platinum solution; With this solution decompression distillation, obtain faint yellow to colourless chlorination four ammonia platinum solid 7.13g.
Adopting model is 353 [M+H]
+EFI mass spectrograph (ESI-MS) carry out ultimate analysis, actual value N%15.60, H%3.45 Pt%55.41; Theoretical value N%15.91, H%3.41 Pt%55.40.
Embodiment 3: take by weighing purity and be 99% 30gMagnus salt, join in the round-bottomed flask, add concentration and be 28% 120ml ammoniacal liquor; Under normal pressure, boiling condition; About 6h that refluxes all disappears to green Magnus salt, faint yellow to colourless chlorination four ammonia platinum solution; With this solution decompression distillation, obtain faint yellow to colourless chlorination four ammonia platinum solid 10.45g.
Adopting model is 353 [M+H]
+EFI mass spectrograph (ESI-MS) carry out ultimate analysis: actual value N%15.99, H%3.47 Pt%55.47; Theoretical value N%15.91, H%3.41 Pt%55.40.
Claims (4)
1. the preparation method of chlorination four ammonia platinum; It is characterized in that: solid Magnus salt is mixed back flow reaction with strong aqua; All disappear until green Magnus salt, obtain faint yellow or colourless chlorination four ammonia platinum solution, obtain faint yellow or colourless chlorination four ammonia platinum solids through underpressure distillation.
2. the preparation method of chlorination four ammonia platinum according to claim 1 is characterized in that: the reactant of employing is a Magnus salt, and its molecular formula is [Pt (NH
3)
4] [PtCl
4], its structural formula is:
3. the preparation method of chlorination four ammonia platinum according to claim 1 is characterized in that: the concentration of strong aqua is 24～28%, and the volume ratio of solid Magnus salt and strong aqua is 1:3～4.
4. the preparation method of chlorination four ammonia platinum according to claim 1 is characterized in that: the pressure of back flow reaction is that normal pressure, time are 6～8 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110223209A CN102328962A (en) | 2011-08-05 | 2011-08-05 | Preparation method of tetramine platinum chloride |
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|---|---|---|---|
| CN201110223209A CN102328962A (en) | 2011-08-05 | 2011-08-05 | Preparation method of tetramine platinum chloride |
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| Publication Number | Publication Date |
|---|---|
| CN102328962A true CN102328962A (en) | 2012-01-25 |
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|---|---|---|---|
| CN201110223209A Pending CN102328962A (en) | 2011-08-05 | 2011-08-05 | Preparation method of tetramine platinum chloride |
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|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104140131A (en) * | 2014-08-20 | 2014-11-12 | 山东铂源药业有限公司 | Preparation method of potassium chloroplatinite |
| CN113173607A (en) * | 2021-05-07 | 2021-07-27 | 内江洛伯尔材料科技有限公司 | Synthesis method of trichloro ammino potassium platinate |
| CN114314701A (en) * | 2021-11-30 | 2022-04-12 | 昆明贵研药业有限公司 | Preparation method of potassium trichloro-ammino platinate and application of potassium trichloro-ammino platinate in preparation of cis-ammonia-water-platinum complex |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07138025A (en) * | 1993-11-12 | 1995-05-30 | Tanaka Kikinzoku Kogyo Kk | Production of tetraammine platinum (ii) dichloride |
| JPH08151216A (en) * | 1994-11-28 | 1996-06-11 | Tanaka Kikinzoku Kogyo Kk | Production of tetraammine-platinum (ii) dichloride |
-
2011
- 2011-08-05 CN CN201110223209A patent/CN102328962A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07138025A (en) * | 1993-11-12 | 1995-05-30 | Tanaka Kikinzoku Kogyo Kk | Production of tetraammine platinum (ii) dichloride |
| JPH08151216A (en) * | 1994-11-28 | 1996-06-11 | Tanaka Kikinzoku Kogyo Kk | Production of tetraammine-platinum (ii) dichloride |
Non-Patent Citations (2)
| Title |
|---|
| :武汉大学化学与分子科学学院实验中心: "《有机化学实验》", 31 August 2004, article "回流", pages: 156 * |
| S.A.COTTON: "《Chemistry of precious metals》", 30 June 1997, article "palladium and platinum", pages: 206 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104140131A (en) * | 2014-08-20 | 2014-11-12 | 山东铂源药业有限公司 | Preparation method of potassium chloroplatinite |
| CN104140131B (en) * | 2014-08-20 | 2015-09-16 | 山东铂源药业有限公司 | A kind of preparation method of potassium chloroplatinite |
| CN113173607A (en) * | 2021-05-07 | 2021-07-27 | 内江洛伯尔材料科技有限公司 | Synthesis method of trichloro ammino potassium platinate |
| CN114314701A (en) * | 2021-11-30 | 2022-04-12 | 昆明贵研药业有限公司 | Preparation method of potassium trichloro-ammino platinate and application of potassium trichloro-ammino platinate in preparation of cis-ammonia-water-platinum complex |
| CN114314701B (en) * | 2021-11-30 | 2023-10-20 | 昆明贵研药业有限公司 | Preparation method of potassium ammonium platinum trichloride and application of potassium ammonium platinum trichloride in preparation of cis-ammonium-water-platinum complex |
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Application publication date: 20120125 |