SU96305A1 - The method of obtaining monomethyl-aminoantipyrin - Google Patents

Description

Limestone methods no.i 4eiiH; i myomethyl-amino-antipyrpic. An intermediary product for the production of the therapeutic drug Analgin, is based on the application of the deficient product, benzene, a dehydrate at a specific consumption (twice oo.Tbnie against the theoretical amount) of the deficient sulphate dilitee.

The predecessor has a c.ie for the ripeHMyniecTBa: the consumption of scarce products is reduced, the equipment is simplified, you magnify the output of the agonimideamine anti-pyrcine and the quality of ana gigi is lost.

According to the method proposed, monometi. G-amino-antigshrin is obtained from sodium c. -1-X-sodium-sulphamine-antipyrine by hethylation with dimethyl sulfate or alkaline somatic sulfuric acid in an organic solvent (chlorobenzene, benzene, toluene, etc.) with temperature of 100-110 °

Example 1, By, 1 learning freedoms Hoif eulfamino-kis, totes from the sodium salt of sulfamino-antipyrine.

1500 l of Na-salt solution of sulfamino-antipyrine, containing about.

.10 12 (1 xg amino-gp-ggiiprina processed:: 3; 11ts niin temperature -1 () - -io 135 kg of KperiKoii ceiiHOii acid.

 in which, 1I: value of L0– kg (90–96), the fate of Agino-acid otde, 1 is taken from the sour, that is, the rest of the p; alignment on the center of the center and passed on to, 1SD ju1tsuuyu stage.

From the acidic mother liquors under ... by siphoning, 1 base of amiponyl type is given in p and m with n}. According to the Ha-salt 4 -, - sodium 1 -su, 1famnno-ait11Pirin (disodium salt).

135 kg of su, 1fam1 no-kps, tota, content of te; 94.5 kg of a | ino-antipyne | zina, exchanged in water (1: 2) and, in the mother liquor from the unreleased: operations; lipif temperature precipitates 182 kg) caustic pat) a. “Dinatropium co, 1b”, which is separated, is discharged from the gullet uterine regimen with oxygen, washed with a small amount of nzolypropyl alcohol and dried P) n temperature 80 ° until its content is 1ag 3-4, 170 kg disodium salt contains 52% a.% n) 1 i-aiti 1iriya.

Example 3. Pohlhchenis monomstil-aminoaithiolnyaa. {Methylation of di 11at1) 11 of one salt with dimethyl sulfate).

170 Ks of dry sunmont is stirred in 280 liters of dry chlorine-isol and 40 Ks of dimethyl sulfate is poured into the mixture. Methylation is carried out for five hours at ipu temperature of 95-100 °. At the end of the Scientific Research Institute of Methylation in I1, 250 l of water and 34 kg of strong sulfuric acid cells were poured into the desired reaction mass, before the acidic reaction to the paper congo.

Maseu is subjected to hydrolysis, heating it for one hour to 100 °; then the colored chlorobenzene solution is separated from the solution containing monomethyl-amino-antipyrine sulfate; The latter is alkalinized to a weakly acid reaction to Congo, treated with a small amount of acetic acid salt, and a small amount of the remaining amino antipyrine is precipitated with benzaldehyde. An aqueous weakly acidic solution of monomethyl-amino-antipyrine, obtained after separation of the benzylidene base (3-4 kg), is alkalinized to a weakly draped reaction (to bromine-cresol purple) and the monomethylamino-antipyrine released to the oil is extracted with 240 l of chlorobenzene. About 300 l of chlorobenzene solution is obtained,

containing monomethyl-amino-antipyrine, which is then treated with formaldehyde bisulfite mixture according to the existing method.

The total yield of myomethyl-aminoactipyrin is 80 kg, i.e., 84.6% of the theory per aMHKo-aHTHnHpvjH.

Example 4. A methylation agent was loaded with:

a) 340 l of chlorobenzene,

b) 170 kg of disodium salt,

c) 72 kg of sodium methyl sulfate (or the corresponding amount of potassium salt).

The mixture is stirred, heated to 100-110 ° and at this temperature methylated for 5-6 hours. Further processing of the methylation product is carried out exactly as in the methylation with dimethyl sulfate.

Subject invention

A method of producing monomethyl-amino-antipyrine, characterized in that monomethyl-amino-antipyrine is obtained from sodium salt of 4-sodium sodium sulfamino-antipyrine by methylation with dimethyl sulfate or an alkaline salt of methyl sulfuric acid in an organic

solvent (chlorobenzene, benzene, toluene, etc.) at a temperature of 100-110 °.