GB1002129A - Organosilicon compounds containing phosphorous - Google Patents

Abstract

The invention comprises silane compounds of the general formula [(CH3)2ZSi(CRR1)3] nR113- nPO where Z is a methyl or hydroxyl group, R and R1 which may be the same or different are hydrogen or alkyl groups containing not more than 4 C atoms or phenyl groups, R11 is an alkyl group containing not more than 6 carbon atoms or is a phenyl group and n is an integer of 1 to 3. The invention further comprises polysiloxanes obtained by hydrolysis of these compounds where Z = OH, alone or with other hydrolysable silanes. The silanes are prepared by reaction of a Grignard reagent with a phosphorus oxyhalide, e.g. POCl3, C6H5POCl2, CH3POCl2 or C2H5POCl2, at 40 DEG to 130 C. in an atmosphere of N2 in presence of a solvent, e.g. lower dialkyl ethers such as diethyl ether, di-n-propyl ether, di-n-butyl ether, tetrahydrofuran or tetrahydropyran. The Grignard reagent is prepared from a gamma-chloro or bromo propyl di- or trimethyl silane, e.g. (CH3)3Si(CH2)3Cl (CH3)3Si(CH2)3BrC6H5(CH3 2Si(CH2)3Cl (CH3)3SiCH2CH(CH3)CH2Cl with magnesium. The compounds where Z is OH are prepared from the corresponding dimethyl phenyl silyl compounds by converting to the dimethylbromosilyl compound and from the corresponding trimethylsilyl compounds by reaction with concentrated sulphuric acid and subsequent treatment with iced water at 10-25 DEG C. and up to about 100 DEG C. Condensation of -OH containing compounds occurs readily on standing. Examples (1)-(4) describe the preparation of tris-(gamma-trimethyl silyl propyl) phosphine oxide and bis-(gamma-trimethyl silyl propyl) phenyl phosphine oxide and the hydroxy compounds derived therefrom and Examples (5)-(8), the preparation of bis-(gamma-trimethyl silyl propyl), methyl phosphine oxide his(gamma trimethyl silyl propyl) ethyl phosphine and their condensation products. Examples (4) and (9) further describe the preparation of mixed condensates.