DE952263C - Process for the preparation of esters of inorganic acids - Google Patents
Process for the preparation of esters of inorganic acidsInfo
- Publication number
- DE952263C DE952263C DEK17163A DEK0017163A DE952263C DE 952263 C DE952263 C DE 952263C DE K17163 A DEK17163 A DE K17163A DE K0017163 A DEK0017163 A DE K0017163A DE 952263 C DE952263 C DE 952263C
- Authority
- DE
- Germany
- Prior art keywords
- esters
- alcoholates
- magnesium
- inorganic acids
- group
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 150000002148 esters Chemical class 0.000 title claims description 11
- 238000000034 method Methods 0.000 title claims description 5
- 150000007522 mineralic acids Chemical class 0.000 title claims description 3
- 238000002360 preparation method Methods 0.000 title description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- 150000002222 fluorine compounds Chemical class 0.000 claims description 6
- 230000000737 periodic effect Effects 0.000 claims description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 4
- 239000011575 calcium Substances 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000011777 magnesium Substances 0.000 claims description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 150000004707 phenolate Chemical class 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052787 antimony Inorganic materials 0.000 claims description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052785 arsenic Inorganic materials 0.000 claims description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000010936 titanium Substances 0.000 claims description 2
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000011541 reaction mixture Substances 0.000 description 3
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical class O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 1
- DJHGAFSJWGLOIV-UHFFFAOYSA-N Arsenic acid Chemical class O[As](O)(O)=O DJHGAFSJWGLOIV-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical class OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- ZMRQTIAUOLVKOX-UHFFFAOYSA-L calcium;diphenoxide Chemical compound [Ca+2].[O-]C1=CC=CC=C1.[O-]C1=CC=CC=C1 ZMRQTIAUOLVKOX-UHFFFAOYSA-L 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- -1 inorganic esters Acids Chemical class 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- KRPXAHXWPZLBKL-UHFFFAOYSA-L magnesium;diphenoxide Chemical compound [Mg+2].[O-]C1=CC=CC=C1.[O-]C1=CC=CC=C1 KRPXAHXWPZLBKL-UHFFFAOYSA-L 0.000 description 1
- XDKQUSKHRIUJEO-UHFFFAOYSA-N magnesium;ethanolate Chemical compound [Mg+2].CC[O-].CC[O-] XDKQUSKHRIUJEO-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-M phenolate Chemical compound [O-]C1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-M 0.000 description 1
- 229940031826 phenolate Drugs 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 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
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/04—Esters of silicic acids
-
- 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
-
- 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
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/02—Boron compounds
- C07F5/04—Esters of boric acids
-
- 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
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/003—Compounds containing elements of Groups 4 or 14 of the Periodic Table without C-Metal linkages
-
- 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
- C07F9/66—Arsenic compounds
- C07F9/68—Arsenic compounds without As—C bonds
Landscapes
- 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)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Verfahren zur Herstellung von Estern anorganischer Säuren Gegenstand des Patents gro 29,9 ist ein Verfahren zur Herstellung von Estern anorganischer Säuren durch Reaktion von Fluoriden. bzw. Komplexfluoräden bestimmter Elemente mit Aluminiumalkoholaten oder Aluminiumphenolaten.Process for the preparation of esters of inorganic acids Subject of the Gro 29.9 patent is a process for the preparation of inorganic esters Acids through the reaction of fluorides. or complex fluorine threads with certain elements Aluminum alcoholates or aluminum phenates.
Es wurde nun weiter gefunden, daß auch die Alkoholate, oder Phenolate der Metalle der Gruppe II a des Periodischen Systems, insbesondere des Magnesiums und Calciums bzw. deren Mischalkoholate oder -phenolate, wie Magnesiumadum.iniumäthylat der Formel Mg [A1(0 C2 H.)41., mit Fluoriden oder Komplexfluoriden@ von Elementen der 3. bis 5. Gruppe des Periodischen Systems, wie Silicium, Titan, Arsen, Bor, Znrkon, Zinn oder Antimon, unter Bildung von Estern der diesen Fluoriden zugehörenden Säuren; reagieren. Solche Ester sind! z. B. Kieselsäureester, Tibansäureesber, Arseniksäureester oder Borsäureester. An Stelle der Phenolate können auch Kresol.ate undä nliche Substitutionsprodukte verwendet werden. Die Reaktion kann. ferner durch Druck beschleunigt werden.It has now been found that the alcoholates, or phenolates of metals of group II a of the periodic table, especially magnesium and calcium or their mixed alcoholates or phenates, such as Magnesiumadum.iniumäthylat of the formula Mg [A1 (0 C2 H.) 41., with fluorides or complex fluorides @ of elements the 3rd to 5th group of the periodic system, such as silicon, titanium, arsenic, boron, Zirconium, tin or antimony, with the formation of esters of the fluorides belonging to these Acids; react. Such esters are! z. B. Silicic acid esters, tibanic acid esters, arsenic acid esters or boric acid esters. Instead of the phenolates, cresolates and similar substitution products can also be used be used. The reaction can. can also be accelerated by pressure.
Die Ester können aus dem Reaktionsgemisch in an sich bekannter Weise isoliert werden, z. B. durch Extraktion mit Lösungsmitteln" Destillation USW. Beispiel i i 6o Gewichtsbeile K2T4 Fs wurden mit 226 Gewichtsteilen Calciumphenolatinnerhalb 1'/2 Stunden bis auf 34o° erhitzt. Das rote Reaktionsprodukt wurde -daraufhin bei 38a° Badtemperatur im Vakuum destilliert, wobei der rote Titansäuretetraphenylester bei 32o bis 330°/i2 mm überging. Anstatt. den Ester aus dem Reaktionsgemisch zu destillieren, ist es vorteilhaft, das Reaktionsgemisch mit Lösungsmitteln, z. B. Benzol, zu extrahieren, wobei durch Abfiltrieren und Einengen der Lösung prächtige bichromatrote Kristalle des Titansäuretetraphenylesters resultieren. Bieäsp*iel 2 57 Gewichtsteile frisch hergiestelltes, ungereinigtes Magnesiumäthylat wurden mit 71 Gewichtsteilen (= 5o"/o, ITberschuß) Na 2SiFs einige -Zeit bis auf 25o° erhitzt. Der K4eselsäuretetraäthylester (Kp. z64°) destillierte ab 22o° in kontinuierlichem Strom ab. Beispiel 3 i30 Gewichtsteile frisch hergestelltes Calciumäthylat wurden mit 14i Gewichtsteilen (= Soo/o Überschuß) Nag Si Fs gemischt und auf 22o bis 25o° erhitzt. Während des Erhitzens destillierte der Kieselsäuretetraäthylester kontinuierlich ab.The esters can be isolated from the reaction mixture in a manner known per se, e.g. B. by extraction with solvents "distillation, etc. Example ii 60 parts by weight of K2T4 Fs were heated with 226 parts by weight of calcium phenate within 1 1/2 hours to 34o °. The red reaction product was then distilled at a bath temperature of 38 ° in vacuo, with the red tetraphenyl titanate instead of distilling the ester from the reaction mixture, it is advantageous to extract the reaction mixture with solvents, e.g. benzene, whereby splendid bichromatic red crystals of the tetraphenyl titanate are obtained by filtering off and concentrating the solution Bieäsp * iel 2 57 parts by weight of freshly produced, unpurified magnesium ethylate were heated with 71 parts by weight (= 50 "/ o, IT excess) Na 2SiFs for some time up to 250 °. The tetraethyl keselate (boiling point 64 °) distilled off in a continuous stream from 220 °. EXAMPLE 3 130 parts by weight of freshly prepared calcium ethylate were mixed with 14 parts by weight (= soo / o excess) Nag Si Fs and heated to 22o to 25o °. During the heating, the tetraethyl silicate distilled off continuously.
B"eisp4e1 4 i07 Gewichtsteile (= Scao/o Übsrschuß) frisch hergestelltes Magnes.iumphenolat wurden mit 32 Gewichtsteilen Nag Si Fs gemischt und 3 Stunden auf Sao bis 32o° erhitzt. Nach Auffangen des Phenolvorlaufs wurde der Kieselsäuretetraphenyles:ter bei 26o bis 265°/i2 mm abdestilliert.B "eisp4e1 4 107 parts by weight (= scao / o excess) freshly prepared Magnesium phenolate was mixed with 32 parts by weight of Nag Si Fs for 3 hours heated to Sao to 32o °. After collecting the phenol forerunner, the silicic acid tetraphenyl became: ter distilled off at 26o to 265 ° / i2 mm.
Werden Magnesiumalkoholate bzw. -ph enolate zur Umsetzung mit den Fluoriden bzw. Komplexfluoriden, der Elemente der 3. bis. 5. Gruppe des Periodischen Systems benutzt, so erlhält man außer darr gewünschten - Estern. als wertvolles Nebenprodukt noch sehr reines Magnesiumfiuoridy das gerade in neuerer Zeit große Bedeutung bei der Vergütung von optischen Gläsern erlangt hat.Are magnesium alcoholates or -ph enolates for implementation with the Fluorides or complex fluorides, the elements of the 3rd to. 5. Group of the periodic System used, one obtains in addition to the desired esters. as valuable By-product still very pure magnesium fluoride, which has recently been great Has gained importance in the compensation of optical glasses.
Die erfindungsgemäß zur Umsetzung benutzten Alkoholate bzw. Phenolate der Elemente der Gruppe Ha des Periodischen Systems haben den besonderen Vorteil; d-aß sie sehr leicht aus dem Metall. und Alkohol bzw. Phenol bei niedrigen Temperaturen: herzustellen sind. So läßt sich. z. B. Calciumalkoholat oder -phenolat schon bei Zimmertemperatur herstellen, während z. B. bei der Herstellung der entsprechenden. Aluminiumverbindungen ein längeres Erhitzen der Alumi:ni:um-Alkohol"Mischu ng und eine vorherige Aktivierung des Aluminiums notwendig ist.The alcoholates or phenates used according to the invention for the reaction the elements of group Ha of the periodic table have the particular advantage; d-ate them very easily from the metal. and alcohol or phenol at low temperatures: are to be produced. So can. z. B. calcium alcoholate or phenolate already at Produce room temperature while z. B. in the manufacture of the corresponding. Aluminum compounds a prolonged heating of the aluminum: ni: um-alcohol "mixture and prior activation of the aluminum is necessary.
Claims (3)
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEK12311A DE910289C (en) | 1951-12-02 | 1951-12-02 | Process for the preparation of esters of inorganic acids |
| DEK17163A DE952263C (en) | 1951-12-02 | 1953-02-24 | Process for the preparation of esters of inorganic acids |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEK12311A DE910289C (en) | 1951-12-02 | 1951-12-02 | Process for the preparation of esters of inorganic acids |
| DEK17163A DE952263C (en) | 1951-12-02 | 1953-02-24 | Process for the preparation of esters of inorganic acids |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE952263C true DE952263C (en) | 1956-11-15 |
Family
ID=33030650
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEK12311A Expired DE910289C (en) | 1951-12-02 | 1951-12-02 | Process for the preparation of esters of inorganic acids |
| DEK17163A Expired DE952263C (en) | 1951-12-02 | 1953-02-24 | Process for the preparation of esters of inorganic acids |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEK12311A Expired DE910289C (en) | 1951-12-02 | 1951-12-02 | Process for the preparation of esters of inorganic acids |
Country Status (1)
| Country | Link |
|---|---|
| DE (2) | DE910289C (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE892439C (en) * | 1951-01-04 | 1953-10-08 | Courtaulds Ltd | Process for the production of cellulose triesters |
-
1951
- 1951-12-02 DE DEK12311A patent/DE910289C/en not_active Expired
-
1953
- 1953-02-24 DE DEK17163A patent/DE952263C/en not_active Expired
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE892439C (en) * | 1951-01-04 | 1953-10-08 | Courtaulds Ltd | Process for the production of cellulose triesters |
Also Published As
| Publication number | Publication date |
|---|---|
| DE910289C (en) | 1954-04-29 |
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