IL42501A - Process for preparing tricyclohexyltin derivatives - Google Patents

Claims (1)

1. WHAT WE CLAIM IS: 1. A process for preparing tricyclohexyltin halide Sn X, in which X is bromine or chlorine, by reaction of a Grignard compound cyclohexylmagnesiurn halide with tin tetrahalide wherein the two reactants are introduced together into a reaction vessel in such a manner that they react from beginning to end always in a ratio of 3 gram-molecules of Grignard compound cyclohexylmagnesiurn halide to 1 gram-molecule of tin tetrahalide. \ 2. A process according to Claim 1, wherein the cyclohexylmagnesiurn halide is introduced into the reaction as a solution of its complex with an aliphatic ether, or tetrahydrofuran or a tertiary amine in a solvent composed of an excess of aliphatic ether or tetrahydrofuran. 3· A process according to Claim 1 , wherein the cyclohexylmagnesium halide is introduced into the reaction as a solution of its complex with an aliphatic ether, or tetrahydrofuran or a tertiary amine in a hydrocarbon having a boiling point between 70 and 150°C. A process accordin to Claim 2 or 3, wherein the aliphatic ether is ethyl ether or the tertiary amine is triethylamine. 5. A process according to Claim 1, wherein the tin tetrahalide is in solution in a hydrocarbon with a boiling point between 70 and 150°C. 6. A process according to Claim or 5» wherein the hydrocarbon used is toluene. 7. A process according to any of Claims 1 to 6, wherein the solutions of the reactants re supplied in predetermined amounts by a discontinuous metnou. 8. A process according to Claim 7» wherein the solutions of the reactants are introduced into the reaction vessel after a hydrocarbon with a boiling point between 70 and 150°C has already been placed therein. 9. A process according to Claim 7 or 8, wherein the solutions of the reactants introduced simultaneously into the reaction vessel in a stoichiometric ratio of J : 1 are kept constantly stirred during the development of the reaction. 10. A process according to Claim i 8 or 9 wherein the reaction mass is kept at a temperature of 25 - 60°C during the addition of the solutions of the reactants. 11. A process according to any of Claims 7 to 10, wherein the addition of the solutions of the reactnats takes place in 15 - 60 minutes. 12. , A procees according to any of Claims 1 to 6 , wherein the solutions of the reactants are fed continuously through metering devices into a mixer and the mixture obtained is passed into a continuous, reaction vessel, the reaction temperature being maintained between 25 and 60°C and the dwell time of the mixture in the reaction vessel being between 1 and 30 minutes. 13. A process according to Claim 12, wherein a hydrocarbon having a boiling point between 70 and 150°C is placed initially in the mixer in an amount occupying from i to £ of the volume thereof. 1^. A process according to Claim 13» wherein the hydrocarbon used is toluene. 15· ' Tricyclrhexyltin halide obtained by a process according to any of Claims 1 to Ik . ( 16. A process for preparing tricyclohexyltin hydroxide, wherein a solution in organic phase of a tricyclohexyltin halide and by-products which is obtained by a process as claimed in any of Claims 1 to 11* is passed dronwise into boiling water or into a stream of steam av.d ie thereafter treated with an aqueous alkaline solution in the hot state. 17· A process for preparing tricyclohexyltin hydroxide, wherein a solution in organic phase of a tricyclohexyltin halide and by-products which is obtained by a process as claimed in any of Claims 1 to 1^ is treated with a jet of superheated steam so as to remove the solvents and is thereafter treated with an aqueous alkaline solution in the hot state. 18. A process according to Claim 16 or 17, wherein the said organic solution is a solution of tricyclohexyltin halide, dicyclohexyltin dihalide and tin tetrahalide (in traces) in a hydrocarbon with a boiling point between 70 and 150°C. 19· A process according to Claim 16 or 7i wherein the tricyclohexyltin halide is tricyclohexyltin chloride and the dicyclohexyltin y dihalide is dicyclohexyltin dichloride, and the hydrocarbon solvent is toluene. 20. A process for preparing tricyclohexyltin hydroxide wherein a tricyclohexhyltin halide as claimed in Claim 15 is hydrolysed by alkali in an aliphatic alcohol with a boiling point above 70°C. 21 . A process according to Claim 20, wherein the said alcohol is tertiary butyl alcohol. 22. A procer ·. p cording to Claim 20 or 21 , wherein the alcohol used in the said hydrolysis is re-useH as such for similar following hydrolyses. 23· Tricyclohexyltin hydroxide obtained by a process as claimed in any of Claims 16 to 22. . . A process for producing tricyclohexyltin halide from dicyclohexyltin dihalide obtained as by-product of the process as claimed in any of Claims 1 to 14, wherein the dicyclohexyltin dihalide and cyclohexylmagnesium halide are introduced simultaneously into a reaction vessel in such manner that they react from beginning to end in a ratio of 1 gram-molecule of cyclohexylmagnesium halide for every gram-molecule h \ of dicyclohexyltin dihalide, the reactants being dissolved in hydrocarbon with a boiling point between 70 and 150°C and in the presence of a complexing agent for the Grignard compound, and the introduction of the reactants taking place in 15 - 60 minutes at a temperature of 25 - 60°C. ^· A process for producing tricyclohexyltin halide substantially as described in any of Examples 1 , 2 and 6. 26. A process for producing tricyclohexyltin hydroxide substantially as described in any of Examples 3, 4 and . COHEN ZEDEK oVSPISBACH P. O. Box 33116 , Tel~.A viv Attorneys for Applicant