METHOD FOR SEPARATION OF RACEMIC 3-(2-METHOXYPHENOXY)-1,2- PROPANEDIOL AND 3-(2-METHYLPHENOXY)-1,2-PROPANEDIOL FOR ENANTIOMERS Russian patent published in 2003 - IPC

Abstract RU 2213724 C1

FIELD: organic chemistry, chemical technology. SUBSTANCE: invention relates to method for separation of racemic 3-(2-methoxyphenoxy)-1,2-propanediol and 3-(2- methylphenoxy)-1,2-propanediol for enantiomers that can be used in pharmaceutical industry in preparing non-racemic medicinal preparations. Racemic diol is enriched a little with one of enantiomers in suitable solvent at temperature 40-60 C to obtain concentrated solution and stirred with graduate cooling to 10-40 C to provide its supersaturation. Then crystalline primer of the same enantiomer is added that is added for enrichment, kept at crystallization point in the range 5- 33 C for 30-60 min, solid precipitate of scalenohedral diol is filtered off that shows the same configuration as a sample of added prime. Then racemic compound is added to mother liquor enriched with the second enantiomer being racemic compound is taken in the amount compensating the separated precipitate, heated to complete dissolution at 40-60 C and then cooled to 10-40 C. Then crystalline primer of enantiomer prevailing in solution is added, kept at stirring at crystallization point in the range 5-33 C, precipitated enriched with the second enantiomer is separated followed repeating indicated process some times. As a rule, benzene, carbon tetrachloride or its mixture with methylene chloride in the ratio 1:1, 40% ethanol aqueous solution and water are used a solvent. Method provides preparing the known drugs in non-racemic form from inexpensive racemic substrates. EFFECT: improved separating method. 2 cl, 1 tbl, 7 ex

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RU 2 213 724 C1

Authors

Bredikhin A.A.

Bredikhina Z.A.

Lazarev S.N.

Sinjashin O.G.

Dates

2003-10-10Published

2002-07-09Filed