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1. (US5210260) Process for obtaining bis(2,4-di-tert-butylphenyl) halophosphites
Note: Texte fondé sur des processus automatiques de reconnaissance optique de caractères. Seule la version PDF a une valeur juridique
We claim:
1. Process for obtaining bis(2,4-di-tert-butylphenyl) halophosphites of the formula in which X is a halogen having an atomic weight of at least 35, which comprises heating a 2,4-di-tert-butylphenyl dihalophosphite of the formula (II) to 130° to 280° C. in the presence of a catalytically active compound containing nitrogen and/or phosphorus and removing the phosphorus trihalide, formed in this way by disproportionation, from the reaction mixture.
2. Process according to claim 1, wherein the removal of the phosphorus trihalide is assisted by passing through a gas which is inert to the reactants.
3. Process according to claim 1 or 2, wherein, by addition of a less than stoichiometric amount of 2,4-di-tert-butylphenol, additional bis(2,4-di-tert-butylphenyl) halophosphite (I) is formed.
4. Process according to claim 3, wherein the 2,4-di-tert-butylphenol is added in an amount of up to 0.9 equivalents per mole of 2,4-di-tert-butylphenyl dihalophosphite.
5. Process according to claim 4, wherein the 2,4-di-tert-butylphenol is added in an amount from 0.3 to 0.6 equivalents per mole of 2,4-di-tertbutylphenyl dihalophosphite.
6. Process according to claim 1, wherein the reaction is carried out without addition of a solvent.
7. Process according to claim 1, wherein the catalyst employed is at least one representative from the group comprising
a) compounds of the formulae (III), (IV), (V) or (VI) in which Y is an element of the fifth main group of the Periodic Table according to Meyer-Mendeleev having an atomic number of 7 to 15, A is an inorganic or organic acid radical, R 1, R 2, R 3 and R 4 are identical or different organic radicals having up to 20 carbon atoms, where two of the radicals R 1 to R 4 or, in the case of the general formula (VI), two or three of the radicals R 1 to R 3 can close to give a cyclic system, optionally with the inclusion of a heteroatom such as oxygen, nitrogen or sulfur, and Z is oxygen or--if Y is phosphorus--alternatively sulfur, two halogen atoms or the group NR 5, where R 5 is R 1 or hydrogen,
b) acid amides and/or
c) compounds from the group comprising mono- to tri-basic organic or inorganic fully amidated acids of tri- or pentavalent phosphorus, whose nitrogen atoms are alkylated by aliphatic radicals having up to 20 carbon atoms and whose organic radicals can contain up to 20 carbon atoms.
8. Process according to claim 7, wherein a tertiary amine is used as the catalyst (III).
9. Process according to claim 1, wherein the catalytically active compound is present in an amount from 0.0001 to 0.1, mol per mole of the 2,4-di-tert-butylphenyl dihalophosphite (II).
10. Process according to claim 1, wherein, to isolate the product (I), residual starting material (II) is subsequently removed by distillation.
11. Process according to claim 7, wherein the reaction is carried out at a temperature from 160° to 230° C.
12. Process according to claim 1, wherein said catalytically active compound is present in a catalytically effective amount which is small, in molar terms, relative to the amount of 2,4-di-tert-butylphenyl dihalophosphite present during said heating step.
13. Process according to claim 12, wherein said catalytically effective amount is about 0.0001 to about 0.1 mol per mole of 2,4-di-tert-butylphenyl dihalophosphite.
14. Process according to claim 13, wherein said catalytically effective amount is about 0.001 to about 0.02 mol per mol of 2,4-di-tert-butylphenyl dihalophosphite.
15. Process according to claim 1, wherein said heating is carried out substantially in the absence of solvent.
16. Process according to claim 15, wherein the compounds present during said heating consist essentially of:
said 2,4-di-tert-butylphenyl dihalophosphite,
a catalytic amount, which is small, in molar terms, relative to said 2,4-di-tert-butylphenyl dihalophosphite, of said catalytically active compound, and
optionally, an amount, less than a stoichiometric amount relative to said 2,4-di-tert-butylphenyldihalophosphite, of 2,4-di-tert-butylphenol.
17. Process according to claim 16, wherein said amount of 2,4-di-tert-butylphenol is present during said heating.