SU323400A1 - METHOD OF OBTAINING 1, B-DICHLOR-4,8 DINITROANTHINO ^ ^ s ^^ '- -' 'tits-n: l.;; - ^ BIBLE _ ::: ^ 111 - Google Patents
METHOD OF OBTAINING 1, B-DICHLOR-4,8 DINITROANTHINO ^ ^ s ^^ '- -' 'tits-n: l.;; - ^ BIBLE _ ::: ^ 111Info
- Publication number
- SU323400A1 SU323400A1 SU1456291A SU1456291A SU323400A1 SU 323400 A1 SU323400 A1 SU 323400A1 SU 1456291 A SU1456291 A SU 1456291A SU 1456291 A SU1456291 A SU 1456291A SU 323400 A1 SU323400 A1 SU 323400A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- obtaining
- dinitroanthino
- bible
- tits
- dichlor
- Prior art date
Links
- 210000002787 Omasum Anatomy 0.000 title 1
- 239000000047 product Substances 0.000 description 5
- LQNUZADURLCDLV-UHFFFAOYSA-N Nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000006396 nitration reaction Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 101710005233 ADGRV1 Proteins 0.000 description 1
- 108060006202 ATM Proteins 0.000 description 1
- RZVHIXYEVGDQDX-UHFFFAOYSA-N Anthraquinone Chemical compound C1=CC=C2C(=O)C3=CC=CC=C3C(=O)C2=C1 RZVHIXYEVGDQDX-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing Effects 0.000 description 1
Description
Изобретение отиоентс к сиособам получени ироизводиых антрахинона, в частности 1,5-дихлор-4,8-диинтроантрахри10на, примен емого в качестве нромежуточного продукта в синтезе аитрахиноиовых красителей.The invention describes the methods of obtaining and producing anthraquinone, in particular, 1,5-dichloro-4,8-diintro-anthracryne, which is used as the intermediate product in the synthesis of nitrahino dyes.
Известен способ иолучеип 1,5-дихлор-4,8диннтроантрахнпоиа иутем нитровани 1,5-дихлорантрахинона азотной кислотой с последующим выделением нелевого нродукта из реакциоииой масс1 известными нриемами и очисткой его нутем многократной перекристаллпзацнн из иитробензола. Однако даже многократна очистка целевого продукта ие позвол ет получить вегцество достаточиой стене н чистоты. По даппым хроматографического анализа красптелп, сиптезнрованные на основе нерекристаллизова1 ного из нитробензола 1,5-дихлор-4,8-диннтроантрахинона, содержат большое количество окрашенных в различные цвета нрпмееей, лншь частично отдел емых перекрнсталлпзацней.The known method is i-type with 1,5-dichloro-4,8 in the form of anthrathramine and the nitration of 1,5-dichlororanthraquinone with nitric acid, followed by separation of the non-nevyl product from the reaction mass1 with the known methods and purification with multiple recrystallized from it and nitrobenzene. However, even repeated purification of the target product does not allow vegetation to be of sufficient wall or purity. According to a chromatographic analysis of the crasptels, which were based on 1,5-dichloro-4,8-dinntroanthraquinone non-recrystallized from nitrobenzene, contain a large number of colored in different colors, which are partially separated by interlacing.
С целью повышени стеиени чистоты 1,5дихлор-4 ,8-дпиитроаитрахинопа ио предлагаемому способу реакииоиную массу, полученную при нитроваинн, фильтруют, осадок промывают концептрпроваиной серной кислотой, водой и сушат.In order to improve the purity of 1.5 dichloro-4, 8-diterroitin, and the proposed method, the reacioine mass obtained with nitroowinn is filtered, the precipitate is washed with sulfuric acid, water and dried.
Пример. В 120 .1/. 94)о-ной серной кнслоiTii , нагретой до 60-ТО С, раствор ют 12 t 1,5-дихлораитрахпиопа. К охлаждеппому до ЗОС раствору при перемешпванпп нрнбавл IOT в течение 20 мин ннтрующую смесь из 6,4 м. 70%-ной азотпой кислоты и 12 мл 94%пой серной кислоты. Перемешивапне продолжают 3 час, после чего реакнионную смесь выдерживают 18 час при комнатной температуре . Продукт нитроваии отфильтровывают и промывают па фильтре 94%-ной ссрпой кислотой (500-600 л;.;) до тех пор, пока проба фпльтрата, смеп1аииа с равным объемом воды , в течение 10 мин не будет давать хлоньевпдиого осадка. Полученный 1,5-дихлор-4,8-дипптроаптрахинои промывают водой до нейгральпой реакпии и сушат при комнатиой температуре . Выход 12 г (75%). /.ма;г: 343 ммк, itic 3,65 (нирндпи).Example. At 120 .1 /. 94) With th-sulfuric sulfur dioxide heated to 60-TO C, 12 t 1,5-dichloroitrachiope are dissolved. By cooling to an AIA solution with an IOT stirrer for 20 minutes, an intrinsic mixture of 6.4 m. Of 70% nitric acid and 12 ml of 94% sulfuric acid. Stirring is continued for 3 hours, after which the reaction mixture is kept for 18 hours at room temperature. The nitro product is filtered and washed on the filter with 94% acidic acid (500-600 l;;) until a sample of the mixture, mixed with an equal volume of water, gives an unstable precipitate for 10 minutes. The resulting 1,5-dichloro-4,8-diptroaptrahinoi is washed with water until neigralpine and dried at room temperature. Yield 12 g (75%). /.ma; g: 343 MMK, itic 3.65 (nirndpi).
П р е д м е т и з о б р е т с и и PREDETE H and o about the and with and
Способ получепи 1,5-дпхлор-4,8-динитроаптрах1 иопа нитровани 1,5-дихлораитрахинона азотной кислотой с выделенпем целевого продукта известными приемами, отличающийс тел1, что, с целью повыишни степени чистоты целевого , реакционную массу, нолучснн 10 нри иитроваг.ии, фнл1) li осадок многократно промывают коицептрированной cepnoii кислотой.The method of obtaining the 1,5-dphlor-4,8-dinitroaptrah 1 of the nitration of 1,5-dichloroitraquinone with nitric acid with extract of the target product by known methods, characterized by the tel1, that, in order to increase the purity of the target, the reaction mass, but 10 nitsititag. , fnl1) li the precipitate is repeatedly washed with co-cepnoii acid.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU323400A1 true SU323400A1 (en) |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4029680A (en) * | 1974-08-03 | 1977-06-14 | Bayer Aktiengesellschaft | Process for the preparation of diamino-dihydroxy anthraquinone disperse dyestuffs |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4029680A (en) * | 1974-08-03 | 1977-06-14 | Bayer Aktiengesellschaft | Process for the preparation of diamino-dihydroxy anthraquinone disperse dyestuffs |
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