CS238792B1 - A method for indicating the progress of diazotization of 2,5-dialkoxy-4-morpholinylaniline by nutylnitrite - Google Patents
A method for indicating the progress of diazotization of 2,5-dialkoxy-4-morpholinylaniline by nutylnitrite Download PDFInfo
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- CS238792B1 CS238792B1 CS84168A CS16884A CS238792B1 CS 238792 B1 CS238792 B1 CS 238792B1 CS 84168 A CS84168 A CS 84168A CS 16884 A CS16884 A CS 16884A CS 238792 B1 CS238792 B1 CS 238792B1
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- morpholinylaniline
- dialkoxy
- diazotization
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- indicating
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Abstract
Způsob sledování průběhu diazotace 2,5-dialkoxy-4-morfolinylanilinu butyl· nitrátem.Method for monitoring the progress of diazotization of 2,5-dialkoxy-4-morpholinylaniline with butyl nitrate.
Description
Vynález řeší způsob sledování diazotace 2,5-dialkoxy-4-morfolinylanilinu. V provozním měřítku se diazotuje aminolátka ňa diazolátku vždy přebytkem cca 10 až 20 % diazotačního činidla, neboť většinou není známa okamžitá koncentrace aminolátky ani koncentrace diazotačnlho činidla, vzhledem k tomu, že butylnitrit je nestálý. Dodaný přebytek diazotačního činidla do reakční smšsi má negativní vliv jak na kvalitu, tak na stabilitu vzniklé diazolátky.The invention provides a method for monitoring diazotation of 2,5-dialkoxy-4-morpholinylaniline. On an industrial scale, the amino compound and diazo compound are always diazotized with an excess of about 10 to 20% of the diazotizing agent, since the immediate concentration of the amino compound and the diazotizing agent concentration are generally unknown, as butylnitrite is unstable. The excess excess diazotizing agent added to the reaction mixture has a negative effect on both the quality and the stability of the diazo compound formed.
Nyní byl nalezen způsob indikace průbšhu diazotáce 2,5-dialkoxy-4-morfolinylanilinu butylnitritem, který je předmětem tohoto vynálezu a jehož podstata spočívá v tom, že přebytek diazotačního činidla ve vodném a acetonovém reakčním prostředí se v bodě ekvivalence indikuje na elektrodovém systému zlatá rotační elektroda nasycená kalomelová elektroda.We have now found a method for indicating the progress of diazotation of 2,5-dialkoxy-4-morpholinylaniline by butyl nitrite according to the present invention, which is based on the fact that an excess of diazotizing agent in an aqueous and acetone reaction medium is indicated at the equivalence point saturated calomel electrode.
Vhodnost použití potenciometrická indikace;je ověřena jak pro diazotaci v roztoku, tak v suspenzi a jak ve vodném tak i acetonovém-prostředí za použití diazotačního činidla jednak vodného roztoku dusitanu sodného £, (NaííO2) = 6 mol/1, jednak samotného butylnitritu. Ve všech případech je možno indikovat nepatrný,'přebytek diazotačního činidla v reakční smšsi. Jedna kapka činidla vpravená do reakční směsi v bodě ekvivalence vyvolá potenciálovou změnu 150 až 200 mV.The suitability of use of the potentiometric indication is verified for both diazotization in solution and suspension and in both aqueous and acetone media using a diazotizing agent on the one hand aqueous sodium nitrite (Na 2 O) = 6 mol / l and on the other hand butylnitrite alone. In all cases, a slight excess of diazotizing agent in the reaction mixture can be indicated. One drop of reagent introduced into the reaction mixture at the equivalence point induces a potential change of 150 to 200 mV.
PříkladExample
Do 150ml kádinky se nalije 100 ml acetonu a 0,5 ml koncentrovaná kyseliny sírové.Pour 100 ml of acetone and 0.5 ml of concentrated sulfuric acid into a 150 ml beaker.
K roztoku se přiaype 1 gram diaza 2,5-dibutoxy-4-morfolinylanilinu a přisype cca 3,75 gramu 2,5-dibutoxy-4-morfolinylanilinsulfátu. Provozní podmínky jsou upraveny do laboratorního měřítka při zachování všech koncentračních poašrů. Diazotace se provádí seaotným butylnitritem z byřety chlazená ledovou drtí. Z počátku se diazotuje po mililitrech v okolí bodu ekvivalence po kapkách.1 gram of diaza 2,5-dibutoxy-4-morpholinylaniline sulfate is added to the solution and about 3.75 g of 2,5-dibutoxy-4-morpholinylaniline sulfate are added. The operating conditions are adjusted to the laboratory scale while maintaining all concentration poaching. The diazotization is carried out with seaot butylnitrite from a burette cooled ice crush. Initially diazotized in milliliters around the equivalence point dropwise.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS84168A CS238792B1 (en) | 1984-01-09 | 1984-01-09 | A method for indicating the progress of diazotization of 2,5-dialkoxy-4-morpholinylaniline by nutylnitrite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS84168A CS238792B1 (en) | 1984-01-09 | 1984-01-09 | A method for indicating the progress of diazotization of 2,5-dialkoxy-4-morpholinylaniline by nutylnitrite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CS16884A1 CS16884A1 (en) | 1985-05-15 |
| CS238792B1 true CS238792B1 (en) | 1985-12-16 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS84168A CS238792B1 (en) | 1984-01-09 | 1984-01-09 | A method for indicating the progress of diazotization of 2,5-dialkoxy-4-morpholinylaniline by nutylnitrite |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS238792B1 (en) |
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1984
- 1984-01-09 CS CS84168A patent/CS238792B1/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| CS16884A1 (en) | 1985-05-15 |
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