DE1121048B - Process for the preparation of boron trialkyls - Google Patents
Process for the preparation of boron trialkylsInfo
- Publication number
- DE1121048B DE1121048B DEK38918A DEK0038918A DE1121048B DE 1121048 B DE1121048 B DE 1121048B DE K38918 A DEK38918 A DE K38918A DE K0038918 A DEK0038918 A DE K0038918A DE 1121048 B DE1121048 B DE 1121048B
- Authority
- DE
- Germany
- Prior art keywords
- boron
- preparation
- alkyl aluminum
- reaction
- trialkyls
- 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.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title description 4
- 229910052796 boron Inorganic materials 0.000 title description 4
- 238000002360 preparation method Methods 0.000 title description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 11
- 125000005234 alkyl aluminium group Chemical group 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- -1 alkyl aluminum halides Chemical class 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- CMAOLVNGLTWICC-UHFFFAOYSA-N 2-fluoro-5-methylbenzonitrile Chemical compound CC1=CC=C(F)C(C#N)=C1 CMAOLVNGLTWICC-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- LALRXNPLTWZJIJ-UHFFFAOYSA-N triethylborane Chemical group CCB(CC)CC LALRXNPLTWZJIJ-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000005662 Paraffin oil Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- KPSZQYZCNSCYGG-UHFFFAOYSA-N [B].[B] Chemical compound [B].[B] KPSZQYZCNSCYGG-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical class Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000375 suspending agent Substances 0.000 description 1
- 239000000725 suspension 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
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/02—Boron compounds
- C07F5/027—Organoboranes and organoborohydrides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Description
Verfahren zur Herstellung von Bortrialkylen Aus dem Journal of the American Chemical Society, Vol. 81 (1959), S. 4794, ist die Umsetzung von Bortrioxyd mit Äthylaluminiumsesquichlorid bekannt, wobei Bortriäthyl jedoch in nur 3,5°/Oiger Ausbeute erhalten wurde. Als borhaltiger Ausgangsstoff muß gewöhnliches handelsübliches Bortrioxyd vorgelegen haben, welches für die Alky]ierung mittels Alkylaluminiumsesquichlorid nicht geeignet ist, was auch durch eigene Versuche bestätigt wurde.Process for the preparation of boron trialkyls From the Journal of the American Chemical Society, Vol. 81 (1959), p. 4794, is the reaction of boron trioxide known with ethyl aluminum sesquichloride, but boron triethyl in only 3.5% Yield was obtained. Ordinary commercially available materials must be used as the starting material containing boron Boron trioxide was present, which was used for the alkylation by means of alkylaluminum sesquichloride is not suitable, which has also been confirmed by our own tests.
Es wurde nun überraschenderweise gefunden, daß man Bortrialkyle in hoher Ausbeute erhält, wenn man ein Bortrioxyd, welches durch Vakuumentwässerung von Borsäure bei Temperaturen zwischen 150 und 250 C hergestellt worden ist, mit Allylaluminiumchloriden, insbesondere Alkylaluminiumsesquichloriden, bei erhöhter Temperatur umsetzt. It has now surprisingly been found that boron trialkyls in high yield is obtained if a boron trioxide is obtained by vacuum drainage has been produced by boric acid at temperatures between 150 and 250 C, with Allyl aluminum chlorides, especially alkyl aluminum sesquichlorides, at increased Temperature converts.
Unter den Begriff Alkylaluminiumchloride fallen Verbindungen, wie Dialkylaluminiumchloride, Alkylaluminiumdichloride, Alkylaluminiumsesquichloride und deren Komplexverbindungen mit Alkalichloriden. The term alkylaluminum chlorides includes compounds such as Dialkyl aluminum chlorides, alkyl aluminum dichlorides, alkyl aluminum sesquichlorides and their complex compounds with alkali chlorides.
Die letzteren haben den Vorteil, daß sie höher erhitzt werden können.The latter have the advantage that they can be heated higher.
Die Reaktion läuft sowohl ohne Verwendung eines indifferenten Lösungs- oder Suspensionsmittels in hoher Ausbeute ab als auch in einem solchen, wie beispielsweise in Mineralöl, Paraffinöl, Decan und anderen Kohlenwasserstoffen oder deren Gemischen sowie höhersiedendem Siliciumtetraalkylen. Die Umsetzung findet gewöhnlich unter Normaldruck statt, doch ist bei der Herstellung von Bortrimethyl die Anwendung eines geringen Überdrucks vorteilhaft. The reaction runs both without the use of an inert solution or suspending agent in high yield as well as in such, such as in mineral oil, paraffin oil, decane and other hydrocarbons or their mixtures and higher-boiling silicon tetraalkylene. The implementation usually takes place under Normal pressure takes place, but in the production of boron trimethyl the use of one is low overpressure advantageous.
Die günstigste Reaktionstemperatur ist der Bereich von 150 bis 250°C.The most favorable reaction temperature is in the range from 150 to 250 ° C.
Beispiel Eine Suspension von 14 Gewichtsteilen Bortrioxyd, welches durch Vakuumentwässerung von Borsäure bei 150 bis 220 C (Ölbad) hergestellt worden ist, in 130 Gewichtsteilen Äthylaluminiumsesquichlorid, (C2H5)3Al2C13, mit einem Chlorgehalt von 48,70/, wurde 4 Stunden auf 200 bis 250 C (Ölbad) erhitzt. Example A suspension of 14 parts by weight of boron trioxide, which by vacuum dewatering of boric acid at 150 to 220 C (oil bath) is, in 130 parts by weight of ethyl aluminum sesquichloride, (C2H5) 3Al2C13, with a Chlorine content of 48.70 /, was heated to 200 to 250 C (oil bath) for 4 hours.
Im Verlauf der Reaktion destillierten 36,1 Gewichtsteile = 92°/o der Theorie an Bortriäthyl ab. Der Reaktionsrückstand war weiß und fest.In the course of the reaction, 36.1 parts by weight = 92% distilled Theory on boron triethyl. The reaction residue was white and solid.
Claims (1)
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEK38918A DE1121048B (en) | 1959-10-15 | 1959-10-15 | Process for the preparation of boron trialkyls |
| GB3302860A GB900614A (en) | 1959-09-26 | 1960-09-26 | Method of producing boron alkyls |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEK38918A DE1121048B (en) | 1959-10-15 | 1959-10-15 | Process for the preparation of boron trialkyls |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE1121048B true DE1121048B (en) | 1962-01-04 |
Family
ID=7221547
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEK38918A Pending DE1121048B (en) | 1959-09-26 | 1959-10-15 | Process for the preparation of boron trialkyls |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE1121048B (en) |
-
1959
- 1959-10-15 DE DEK38918A patent/DE1121048B/en active Pending
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