PL435B1 - The method of obtaining cyanamides of a-halogenated acids. - Google Patents
The method of obtaining cyanamides of a-halogenated acids. Download PDFInfo
- Publication number
- PL435B1 PL435B1 PL435A PL43520A PL435B1 PL 435 B1 PL435 B1 PL 435B1 PL 435 A PL435 A PL 435A PL 43520 A PL43520 A PL 43520A PL 435 B1 PL435 B1 PL 435B1
- Authority
- PL
- Poland
- Prior art keywords
- cyanamides
- obtaining
- halogenated acids
- acids
- cyanamide
- Prior art date
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- 239000002253 acid Substances 0.000 title claims description 6
- 150000001912 cyanamides Chemical class 0.000 title claims description 5
- 238000000034 method Methods 0.000 title claims description 3
- 150000007513 acids Chemical class 0.000 title claims 3
- 150000004820 halides Chemical class 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000007900 aqueous suspension Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- BDNKAUXMHAPADE-UHFFFAOYSA-N 2-bromo-2-ethylbutanoyl chloride Chemical compound CCC(Br)(CC)C(Cl)=O BDNKAUXMHAPADE-UHFFFAOYSA-N 0.000 description 3
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 3
- -1 calcium nitride Chemical class 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- LUTZMJZHVATZQM-UHFFFAOYSA-N 2-bromo-2-ethylbutanoyl bromide Chemical compound CCC(Br)(CC)C(Br)=O LUTZMJZHVATZQM-UHFFFAOYSA-N 0.000 description 1
- MVXMNHYVCLMLDD-UHFFFAOYSA-N 4-methoxynaphthalene-1-carbaldehyde Chemical compound C1=CC=C2C(OC)=CC=C(C=O)C2=C1 MVXMNHYVCLMLDD-UHFFFAOYSA-N 0.000 description 1
- ZAFIASFVHZLVPF-UHFFFAOYSA-N CCC(Br)(CC)C(=O)NC#N Chemical compound CCC(Br)(CC)C(=O)NC#N ZAFIASFVHZLVPF-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- KXZJHVJKXJLBKO-UHFFFAOYSA-N chembl1408157 Chemical compound N=1C2=CC=CC=C2C(C(=O)O)=CC=1C1=CC=C(O)C=C1 KXZJHVJKXJLBKO-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Description
Stwierdzono, ze przez dzialanie halo¬ genków kwasów a-halogenizowanych na cjanamidki metali w roztworze wodnym, lub zawiesinie, mozna dojsc do cjana- midków kwasów a-halogenizowanych z doskonala wydajnoscia.Przy uzyciu tego sposobu daja sie stosowac techniczne sole cjanamidu, np. kupny cjanamidek sodu lub wapna (azo¬ tek wapnia) z równie dobrym skutkiem, jak najczystsze sole.Stosowanie trudno — lub nierozpu¬ szczalnych soli metalicznych, jak to srebra, miedzi, olowiu i t. p. soli w za¬ wiesinach wodnych nie jest specjalnie korzystnem.Przyklad.Do roztworu 18 — 20 czesci (troche wiecej niz 2 czast.) technicznego cjana- midku sodu o mniej wiecej 95% NH2CN, w 80 cz. wody dolewa sie powoli przy ciaglem mieszaniu 42,7 cz. chlorku dwu- etylo-bromo-acetylu lub zamiast niego 51,6 cz. bromku dwuetylo-bromo-acetylu (2 czast.). Celowem jest utrzymywanie temperatury przy 30°. O ile silniej ozie¬ bic, to czesto krystalizuje sie wieksza czesc soli sodowej dwuetylo-bromo-ace- tylocjanamidu. O ile podniesc tempera¬ ture wyzej, to utrudnia sie prace parami chlorowców; jednak wplyw na przebieg reakcji nie daje sie tu zauwazyc.Do utworzonego przezroczystego roz¬ tworu dolewa sie rozcienczony kwas siarkowy lub solny, tak dlugo, jak dlugo tworzy sie jeszcze oleista wydzielina i dopóki papierek kongo pokazuje mocna, i czysta reakcje.Wydziela sie gesty olej, który do dalszego uzytku, przy którym niewielkazawartosc wody nie szkodzi, jest zupel¬ nie wystarczajaco czysty.Wydajnosc cjanamidku dwuetylo-bn mo-acetylu w postaci bezwodnej wynosi, obliczona na chlorek dwuetylo-bromo- acetylu, okolo 85 — 90%.Zamiast cjanamidku sodu moze byc uzyty, np. cjanamidek wapnia.O ile zamienic w przykladzie chlorek dwuetylo-bromo-acetylu na równowazne ilosci halogenidków kwasu bromowa- lerjanowego, to otrzymuje sie w ten sam sposób, z bardzo dobremi wydaj- nosciami, odpowiednie cjanamidki bro- mowalerylu. PLIt has been found that by the action of α-halogenated acid halides on metal cyanamides in an aqueous solution or suspension, it is possible to obtain α-halogenated acid cyanides with excellent efficiency. With this method, technical cyanamide salts, e.g. Sodium or lime cyanamide (calcium nitride) with as good effect as the purest salts. The use of hard - or insoluble metallic salts such as silver, copper, lead, etc. in aqueous slurries is not particularly advantageous. For a solution of 18 - 20 parts (a little more than 2 parts) technical sodium cyanide with about 95% NH2CN, 80 parts water is added slowly while stirring continuously, 42.7 parts. diethyl-bromo-acetyl chloride or instead 51.6 p. diethyl-bromo-acetyl bromide (2 times). It is a good idea to keep the temperature at 30 °. If it is cooled more often, most of the sodium salt of the diethyl-bromo-acetyl cyanamide crystallizes. If the temperature is raised higher, it is difficult to work with halogen vapors; However, the effect on the course of the reaction is not noticeable here. Dilute sulfuric or hydrochloric acid is added to the resulting clear solution as long as an oily discharge is still formed and the congo paper shows a strong and clear reaction. The yield of diethylbn-monoacetyl cyanamide in anhydrous form, calculated as diethylbromoacetyl chloride, is approximately 85-90% for further use, where a small amount of water does not harm, and is completely pure. Sodium sodium can be used, e.g. calcium cyanamide. If, in the example, diethyl-bromo-acetyl chloride is replaced with an equivalent amount of bromovaleryl acid halide, the corresponding bromovaleryl cyanamide is obtained in the same way with very good yield . PL
Claims (1)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| PL435B1 true PL435B1 (en) | 1924-08-30 |
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