PL78808B2 - - Google Patents

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Publication number
PL78808B2
PL78808B2 PL14925471A PL14925471A PL78808B2 PL 78808 B2 PL78808 B2 PL 78808B2 PL 14925471 A PL14925471 A PL 14925471A PL 14925471 A PL14925471 A PL 14925471A PL 78808 B2 PL78808 B2 PL 78808B2
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PL
Poland
Prior art keywords
aqueous
solution
nitrile
organic
organic solvent
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Application number
PL14925471A
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Polish (pl)
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Priority to PL14925471A priority Critical patent/PL78808B2/pl
Publication of PL78808B2 publication Critical patent/PL78808B2/pl

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Pyridine Compounds (AREA)

Description

Przez schlodzenie lugów poreakcyjnych do temperatury pokojowej (25°C) krystalizowano 45% amidu powstalego w reakcji, dalsze schlodzenie lugów do 0°C pozwolilo wykrystalizowac jeszcze 25% amidu. Krysztaly oddzielono przez filtrowanie i przemyto acetonem. Pozostale 30% amidu wydzie¬ lono przez odparowanie roztworu. Ogólem otrzymano 135 g amidu co odpowiada 73% przemianie nitrylu na amid.. Amid mial temperature topnienia 126,9—128,6°C. Po syntezie 65% jonowymiennych grup katalizatora zablokowane jest anionami nikotynianowymi, które stanowia 1,2% wsadu calkowitego. PL PLBy cooling the reaction liquors to room temperature (25 ° C), 45% of the amide formed in the reaction was crystallized, further cooling of the liquors to 0 ° C allowed a further 25% of the amide to crystallize out. The crystals were separated by filtration and washed with acetone. The remaining 30% of the amide was isolated by evaporation of the solution. A total of 135 g of amide was obtained corresponding to 73% conversion of the nitrile to the amide. The amide had a melting point of 126.9-128.6 ° C. After synthesis, 65% of the ion-exchange groups of the catalyst are blocked with nicotinate anions, which constitute 1.2% of the total input. PL PL

Claims (5)

1. Zastrzezenia patentowe 1. Sposób otrzymywania amidu kwasu nikotynowego z 3-cyjanopirydyny przez niepelna hydrolize nitrylu tego kwasu przy uzyciu anionitów silnie zasadowych, znamienny tym, ze hydrolize prowadzi sie w roztworze wodno-organicznym zawierajacym rozpuszczalnik organiczny mieszajacy sie z woda przepuszczajac roztwór w temperaturze 30-60°C przez warstwe katalizatora w postaci jonitu, po czym mieszanine poreakcyjna oziebia sie i powstale krysztaly wydziela sie przez wirowanie lub saczenie.1. Claims 1. The method of obtaining nicotinic acid amide from 3-cyanopyridine by incomplete hydrolysis of the nitrile of this acid with strongly basic anion exchangers, characterized in that the hydrolysis is carried out in an aqueous-organic solution containing an organic solvent mixed with water by passing the solution at a temperature of 30-60 ° C through the catalyst layer in the form of ion exchanger, after which the post-reaction mixture is cooled and the formed crystals are separated by centrifugation or filtration. 2. Sposób wedlug zastrz. 1, znamienny tym, ze wodnoorganiczny roztwór nitrylu przepuszcza sie przez warstwe jonitu poddanego uprzednio niepelnej regeneracji.2. The method according to claim The method of claim 1, characterized in that the aqueous-organic nitrile solution is passed through the layer of previously incomplete regeneration ion exchanger. 3. Sposób wedlug zastrz. 1 lub 2, znamienny tym, ze stosuje sie wodnoorganiczny roztwór nitrylu zawiera¬ jacy 1—8 moli wody na 1 mol nitrylu.3. The method according to p. A process as claimed in any one of the preceding claims, characterized in that an organo-aqueous nitrile solution is used containing 1 to 8 moles of water per mole of nitrile. 4. Sposób wedlug zastrz. 1 lub 2 lub 3, znamienny tym, ze stosuje sie wodno-organiczny roztwór zawiera¬ jacy 1—15 objetosci rozpuszczalnika organicznego na jedna objetosc wody.4. The method according to p. A process as claimed in any one of the preceding claims, characterized in that an aqueous-organic solution is used containing 1 to 15 volumes of organic solvent per volume of water. 5. Sposób wedlug zastrz. 1 lub 2, lub 3 lub 4, znamienny tym, ze jako rozpuszczalnik organiczny stosuje sie aceton lub nizsze alkohole alifatyczne.KI. 12p, 1/01 78 808 MKPC07d 31/44 100 90 C3 c 10 ^ 70 C ^ 1 O E n 50 SO 5 6 Fio I 10 u T(qodzj Prac. Poligraf. UP PRL T.P.Zam. 208/75 Naklad 120+18 Cena 10 zl PL PL5. The method according to p. A process as claimed in claim 1 or 2, or 3 or 4, characterized in that acetone or lower aliphatic alcohols are used as the organic solvent. 12p, 1/01 78 808 MKPC07d 31/44 100 90 C3 c 10 ^ 70 C ^ 1 OE n 50 SO 5 6 Fio I 10 u T (qty of work. Printing UP PRL TP Order 208/75 Mintage 120 + 18 Price PLN 10 PL PL
PL14925471A 1971-07-06 1971-07-06 PL78808B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL14925471A PL78808B2 (en) 1971-07-06 1971-07-06

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PL14925471A PL78808B2 (en) 1971-07-06 1971-07-06

Publications (1)

Publication Number Publication Date
PL78808B2 true PL78808B2 (en) 1975-06-30

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Application Number Title Priority Date Filing Date
PL14925471A PL78808B2 (en) 1971-07-06 1971-07-06

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PL (1) PL78808B2 (en)

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