http://rdf.ncbi.nlm.nih.gov/pubchem/patent/GB-787180-A

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http://rdf.ncbi.nlm.nih.gov/pubchem/patentcpc/C07F7-003
classificationIPCInventive http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C29-70
http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07F7-00
http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07C31-28
filingDate 1954-06-17-04:00^^<http://www.w3.org/2001/XMLSchema#date>
inventor http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_3d692c63c38e57fe3ffc85551d018db0
publicationDate 1957-12-04-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber GB-787180-A
titleOfInvention Improvements in or relating to the preparation of metal alcoholates
abstract <PICT:0787180/IV (b)/1> Metal alcoholates are obtained by reacting a tertiary alcohol, allylic alcohol, or b -keto alcohol with the ammonia addition product of a halide of a metal having a valency of at least 3 and an atomic number greater than 12 and less than 57, said addition product containing at least one nitrogen atom for each atom of halogen in said halide. Specified metals are titanium, zirconium, iron, arsenic, antimony, tin, and aluminium and specified alcohols include tert.-butyl and tert-amyl alcohols, 1-methyl cyclopentanol, triphenyl carbinol, allyl alcohol, acetyl carbinol, 1-aceto propyl alcohol, and 1-acetobutyl alcohol. It is preferred to use the chlorides of titanium, zirconium, iron, antimony or tin but other halides, e.g. the bromides and iodides of these metals can also be used. The reaction is preferably carried out at a temperature of at least 40 DEG C., e.. aat from 40 DEG C. up to the boiling-point of the alcohol used. The ammonia addition product may be formed by passing anhydrous ammonia into a solution of the halide reactant, e.g. titanium tetrachloride, in an inert organic solvent and then mixed with the alcohol and the mixture heated to form the metal alcoholate. In the Figure, the metal chloride, e.g. titanium tetrachloride, is dissolved in a suitable solvent, e.g. cyclohexane, n-heptane, benzene, toluene, or xylene, in the storage vessel 1 and the solution passed to a mixing zone 7 where it mixes with a solution formed by passing anhydrous ammonia from conduit 9 into a solvent of the same type from storage vessel 2. The ammonia solution becomes homogeneous in the mixing conduit 8 and is injected into the stream of metal halide solution which is being discharged into the zone 7 where the mixing is very rapid. The alcohol reactant which may be heated, if desired, is fed from vessel 3 through line 6 into the discharge line 10 which discharges the reaction mixture into a heated baffled digestion chamber 11 provided with heating coils 12, an outlet 13 and a refluxing tower 14. The ammonium chloride crystals formed in the reaction grow to a filterable size in the digestion chamber and escape of excess ammonia and refluxing of solvent is effected by means of the column 14 and outlet 15. Examples are given for the production from the corresponding alcohol and metal chloride-ammonia addition product of (1) tertiary butyl titanate; (2) tertiary amyl titanate; (3) tertiary butyl antimonite; and (4) the ferric alcoholate derived from tertiary butyl alcohol. The ammonia-metal chloride addition products formed in these examples are stated to have the approximate compositions TiCl48NH3, SbCl3.3NH3 and FeCl35NH3 (or FeCl36NH3). Specification 479,470 is referred to.
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