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
  • C07F5/06—Aluminium compounds
  • C07F5/061—Aluminium compounds with C-aluminium linkage
  • C07F5/064—Aluminium compounds with C-aluminium linkage compounds with an Al-Halogen linkage

Definitions

• the present invention relates to a process for the production of an aluminium alkyl sesquichloride from metallic aluminium and the corresponding alkyl chloride.
• aluminium alkyl sesquichloride is any mixture of an aluminium dialkyl chloride and an aluminium alkyl dichloride, the alkyl groups being the same in both compounds.
• aluminium ethyl sesquichloride is a mixture of the two compounds having the formula Al(C H .Cl and Al(C I-l ).Cl
• aluminium alkyl sesquichlorides consist of equimolar proportions of the two components.
• An object of the present invention is to provide an improved process for the production of aluminium alkyl sesquichlorides in which the above features can all be eliminated.
• the process for the production of an aluminium alkyl sesquichloride from the reaction 'of aluminium with an alkyl chloride comprises reacting the aluminium with the alkyl chloride in the presence of a reaction initiator comprising a mixture of anhydrous aluminium chloride and an aluminium alkyl halide.
• the aluminium used in the reaction can be in any convenient form. In order to increase the reaction rate it is best to provide as large a surface area of aluminium in the reaction mixture as possible and consequently aluminium turnings or powder are particularly useful. However, there is no need to prepare or store the aluminium in a non-oxidising atmosphere. If desired the aluminium can be present as an alloy with another metal or metals which do not interfere with the reaction, e.g. magnesium.
• the alkyl chloride is chosen so that the desired aluminium alkyl sesquichloride is obtained.
• the most useful aluminium sesquichlorides are those derived from lower alkyl groups, i.e. alkyl groups containing not more than four carbon atoms (methyl, ethyl, propyl, butyl, etc), and the process of the present invention is partic- 2,903,469 Patented Sept. 8, 1959 ularly suited for their manufacture.
• the preferred aluminium alkyl sesquichloride is aluminium ethyl sesquichloride which is readily manufactured by the process of the present invention from aluminium and ethyl chloride.
• One component of the reaction initiator mixture is an aluminium alkyl halide.
• This may be an aluminium dialkyl halide or an aluminium alkyl dihalide. Any such compound can be employed, but it is preferred that the alkyl group or groups shall correspond to those in the aluminium alkyl sesquichloride it is desired tomanufacture.
• an aluminium alkyl chloride can be employed and thus the product cannot become contaminated with compounds containing halide atoms other than chlorine.
• a particularly useful component of the reaction initiator mixture is the aluminium alkyl sesquichloride which it is desired to produce.
• the proportion of reaction initiator present in the reaction mixture can be varied considerably because very small amounts initiate the reaction and large amounts have no deleterious effects upon it. Most suitably the total amount of aluminium chloride and aluminium alkyl halide should be in excess of 2% by Weight of the reaction mixture if good initial reaction rates are to be obtained.
• the proportion of aluminium chloride to aluminium alkyl halide .inthe mixture forming the reaction initiator can similarly be varied considerably but, most suitably, one part by weight of aluminium chloride is used in conjunction with at least 0.5 part by Weight of the aluminium alkyl halide. Preferably approximately equal proportions by weight of the two components are used to form the reaction initiator.
• the process according to the present invention can be carried out at atmospheric pressure and is thus a considerable improvement on some of the prior art processes. .If desired super-atmospheric pressures can be employed but this is unnecessary and good yields can beattained usingsimple, non-pressure apparatus.
• the reaction of alumini um with an alkyl chloride under the conditions of the present invention can be brought about at normal ambient temperatures, e.g. 20 C., but preferably the reaction mixture is maintained at at least 50 C.
• the reaction is exothermic and consequently it is not necessary to heat the reaction mixture once the reaction has commenced.
• the process of the present invention can be carried out using either an excess of aluminium or an excess of the alkyl chloride.
• an excess of aluminium is employed because it is easier to recover from the reaction mixture for re-use than an excess of the alkyl chloride.
• the reaction is carried out by mixing the aluminium with the initiator mixture in an atmosphere of an inert gas such as nitrogen, for instance, at a temperature between 50 and C. and then adding the alkyl halide whereupon the reaction immediately begins.
• an inert gas such as nitrogen
• the reaction mixture is held under reflux conditions so that any alkyl halide which vapourises before reacting is condensed and returned to the reaction vessel.
• the lower alkyl chlorides have low boiling points, for example ethyl chloride boils at about 12 C. under atmospheric pressure, and consequently any reflux condensers and the like should be operated with a suitably cooled cooling liquid.
• the reaction is initiated by the presence ab initio of the mixture of aluminium chloride and an Example 1 Aluminium flitters (27 parts) and powdered aluminium chloride parts) are placed in a reaction vessel under nitrogen. Molten aluminium ethyl di-iodide (5 parts) is added, and the mixture heated to about 70 C. Cooled ethyl chloride (96 parts) is added dropwise and maintained under reflux by a condenser carrying cooling liquid at 30 C. Reflux ceases almost entirely after 4 hour. The mixture is heated a little longer, cooled and distilled under reduced pressure caused by a water pump. A good yield of aluminium ethyl sesquichloride is produced.
• Example 2 The process described in Example 1 is followed using 5 parts of aluminium ethyl sesquichloride in place of the aluminium ethyl di-iodide to form the reaction initiator with the aluminium chloride. Again a good yield of aluminium ethyl sesquichloride is obtained.
• Example 3 By proceeding along the lines set forth in Example 1 but replacing the aluminium ethyl di-iodide by a corresponding quantity of aluminium ethyl di-chloride, a similar good yield of aluminium ethyl sesquichloride is obtained.
• Example 4 By proceeding along the lines set forth in Example 1, but replacing the aluminium ethyl di-iodide by the corresponding quantity of aluminium methyl di-chloride and also replacing the ethyl chloride by the corresponding quantity of methyl chloride, the aluminium methyl sesquichloride is obtained.
• the corresponding propyl and butyl derivatives may be obtained by using the corresponding aluminium propyl and butyl di-iodide (or di-chloride) respectively and, if desired, the corresponding propyl or butyl chloride, in lieu of the aluminium ethyl di-iodide and ethyl chloride used in Example 1.
• aluminium alkyl halide initiator is a chloride
• reaction initiator consists of a mixture of aluminium chloride with the aluminium sesquichloride to be produced.
• reaction initiator consists of approximately equal proportions by weight of aluminium chloride and the aluminium alkyl halide.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
• Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)

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• 0
  • NL NL99959T patent/NL99959C/xx active
  • BE BE559506D patent/BE559506A/xx unknown
• 1956
  • 1956-07-26 GB GB23087/56A patent/GB800615A/en not_active Expired
• 1957
  • 1957-06-27 DE DED25862A patent/DE1059450B/de active Pending
  • 1957-07-15 US US671735A patent/US2903469A/en not_active Expired - Lifetime
  • 1957-07-22 FR FR1183714D patent/FR1183714A/fr not_active Expired

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