FIELD: organic chemistry, chemical technology.
SUBSTANCE: invention relates to the improved method for preparing 2,3,4-trimethoxybenzaldehyde used as an intermediate substance for synthesis of medicinal preparations. Method involves interaction of 1,2,3-trimethoxybenzene with dimethylformamide and phosphorus oxychloride and treatment of reaction mixture with water. Reaction is carried out at 80-85 C and product is isolated by either extraction with organic solvent and washing out extract with alkali and sodium chloride aqueous solutions successively, evaporation of solvent and diluting a residue with aliphatic solvent or by crystallization in treatment with water directly, filtering off crystals, their washing out with water and re-pulping crystals in water. Proposed method allows elimination of vacuum-rectification and to obtain the end product with the content 99.5% and the yield about 75%.
EFFECT: improved preparing method, enhanced purity and yield.
3 ex
Title | Year | Author | Number |
---|---|---|---|
METHOD FOR PREPARING 2,3,4-TRIMETHOXYBENALDEHYDE | 2002 |
|
RU2236397C1 |
METHOD FOR PREPARING 1-(2,3,4-TRIMETHOXYBENZYL)-PIPERAZINE DIHYDROCHLORIDE | 2002 |
|
RU2234501C1 |
0 |
|
SU450411A3 | |
0 |
|
SU484690A3 | |
0 |
|
SU451246A3 | |
0 |
|
SU507236A3 | |
0 |
|
SU439092A3 | |
0 |
|
SU220264A1 | |
1S,3R - 2,2 - DIMETHYL -3(2-METHYL -2- OXYPROPYL) -CYCLOPROPANECARBONITRILE AS INTERMEDIATE COMPOUND IN SYNTHESIS OF PYRETHROID INSECTICIDE OF DELTAMETRINE AND METHOD FOR PRODUCTION OF INTERMEDIATE COMPOUND | 1989 |
|
RU1679761C |
0 |
|
SU473361A3 |
Authors
Dates
2004-08-20—Published
2003-03-25—Filed