METHOD OF SYNTHESIS OF BIS-[(4-HYDROXYPHENYL)ALKYL]-SULFIDES Russian patent published in 1995 - IPC

Abstract SU 1658601 A1

FIELD: organic chemistry, sulfide derivatives. SUBSTANCE: product: bis-[(4-hydroxyphenyl)alkyl]-sulfides of the general formula where a) R1=R2-tert. -butyl, R3=H,, n 1-3, or b) R1=R2-tert.-butyl, R5=CH3,, n 2, or c) R1 tert.-butyl, R2=R3=H,, n 1-2; d) R1 tert.-butyl, R2=H,, R3=CH3,, n 2. Synthesis is carried out by chlorination of corresponding alcohol with PCl5 or POCl3 in the presence of dimethylformamide at their molar ratio (1.8-2):1:2, at 90-100 C followed by treatment of reaction mass with alkaline, sulfidizing with sodium sulfide at its molar ratio to prepared chloride (1.0-1.5):2 in alcohol (preferably to take KOH at concentration 0.05-1 mole per 1 mole parental alcohol), at boiling or in dimethylformamide (preferably to take NaOH or KOH as an aqueous solution at concentration 2.3-2.8 mole per 1 mole alcohol) in water presence at concentration 10-15 wt.-% of total dimethylformamide content and water at 70-90 C. Under these conditions the yield of the end product is increased from 79-83% to 85-89% in alcohol and from 78-84% to 93-94% in dimethylformamide. The content of basic substance is increased from 91-94% to 97-98% EFFECT: improved selectivity of process, elimination of by-side processes. 3 cl, 2 tbl

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SU 1 658 601 A1

Authors

Prosenko A.E.

Markov A.F.

Pinko P.I.

Krysin A.P.

Koptjug V.A.

Dates

1995-10-20Published

1989-10-27Filed