CS238792B1 - Method of indication of diazotation of 2,5-dialcoxy-4-morpholinylaniline by butylnitrite - Google Patents
Method of indication of diazotation of 2,5-dialcoxy-4-morpholinylaniline by butylnitrite Download PDFInfo
- Publication number
- 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
- Authority
- CS
- Czechoslovakia
- Prior art keywords
- morpholinylaniline
- butylnitrite
- diazotation
- indication
- dialcoxy
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 5
- JQJPBYFTQAANLE-UHFFFAOYSA-N Butyl nitrite Chemical compound CCCCON=O JQJPBYFTQAANLE-UHFFFAOYSA-N 0.000 title claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000006193 diazotization reaction Methods 0.000 claims description 3
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 2
- 239000012429 reaction media Substances 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 238000012544 monitoring process Methods 0.000 abstract description 2
- 229910002651 NO3 Inorganic materials 0.000 abstract 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 abstract 1
- 239000011541 reaction mixture Substances 0.000 description 3
- ONLYZWBOMYPZPY-UHFFFAOYSA-N (2,5-dibutoxy-4-morpholin-4-ium-4-ylphenyl)azanium;sulfate Chemical compound OS(O)(=O)=O.C1=C(N)C(OCCCC)=CC(N2CCOCC2)=C1OCCCC ONLYZWBOMYPZPY-UHFFFAOYSA-N 0.000 description 2
- -1 amino compound Chemical class 0.000 description 2
- 150000008049 diazo compounds Chemical class 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000010288 sodium nitrite Nutrition 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Způsob sledování průběhu diazotace 2,5-dialkoxy-4-morfolinylanilinu butyl· nitrátem.Method of monitoring the progress of diazotation 2,5-dialkoxy-4-morpholinylaniline 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 | Method of indication of diazotation of 2,5-dialcoxy-4-morpholinylaniline by butylnitrite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS84168A CS238792B1 (en) | 1984-01-09 | 1984-01-09 | Method of indication of diazotation of 2,5-dialcoxy-4-morpholinylaniline by butylnitrite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CS16884A1 CS16884A1 (en) | 1985-05-15 |
| CS238792B1 true CS238792B1 (en) | 1985-12-16 |
Family
ID=5333362
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS84168A CS238792B1 (en) | 1984-01-09 | 1984-01-09 | Method of indication of diazotation of 2,5-dialcoxy-4-morpholinylaniline by butylnitrite |
Country Status (1)
| Country | Link |
|---|---|
| CS (1) | CS238792B1 (en) |
-
1984
- 1984-01-09 CS CS84168A patent/CS238792B1/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| CS16884A1 (en) | 1985-05-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Jenkins et al. | Brucine Method for the Determination of Nitrate in Ocean, Estuarine, and Fresh Waters. | |
| Light | Standard solution for redox potential measurements | |
| Chow et al. | Determination of nitrate in sea water | |
| CS238792B1 (en) | Method of indication of diazotation of 2,5-dialcoxy-4-morpholinylaniline by butylnitrite | |
| Elofson et al. | Amperometric Titration with Diazotized Aromatic Amines | |
| Fogg et al. | Flow injection voltammetric determination of hypochlorite and hypobromite as bromine by injection into an acidic bromide eluent and the indirect determination of ammonia and hydrazine by reaction with an excess of hypobromite | |
| Navratilova et al. | Differential-pulse voltammetric determination of molybdenum in nitrate medium in the presence of 8-hydroxyquinoline | |
| Itikawa et al. | Simplified manufacture and histochemical use of the Schiff reagent | |
| Vytřas et al. | Ion-selective electrodes in titrations involving azo-coupling reactions | |
| CN102590317A (en) | PH composite electrode method for measuring content of nitrite ions in solution | |
| SU1522078A1 (en) | Paste for corrosion resistance of metal materials | |
| Kudo et al. | Complex Formation of Oxonium Ion with 18-Crown-6 and 24-Crown-8 Derivatives in a Nitrobenzene Solution Saturated with Water | |
| Reynolds | The reaction between potassium ferrocyanide and iodine in aqueous solutions | |
| RU2075075C1 (en) | Method of separately determining phenol and formaldehyde in aqueous media | |
| JPS6215261A (en) | Removal of excessive nitrite in diazotizing solution | |
| JPS5610255A (en) | Bilirubin detecting test piece | |
| SU767033A1 (en) | Method of amperomatric determination of chromium | |
| CS238795B1 (en) | Method of determining of 2,5-dialcoxy-4-morpholinylbendiazone compositions | |
| Owen et al. | The Elimination of Liquid Junction Potentials. III. Comparison of the Silver—Silver Chloride and Silver—Silver Bromide Electrodes at 25° | |
| Al-Hajjaji | Polarographic reduction of 2, 4, 6-trinitrobenzene-1-sulphonic acid and some 2, 4, 6-trinitrophenyl-amino acid derivatives | |
| Vytrˇas et al. | Ion-selective electrodes in titrations involving azo-coupling reactions | |
| Katiyar | Kinetic Investigations of the Reaction of Brilliant Green with Alkalies. Influence of Ionic Strength | |
| SU963949A1 (en) | Process for preparing indicator composition for detecting phosphine in air | |
| SU1296913A1 (en) | Ferment electrode for determining concentrations of thiocholine ethers | |
| Karlovský et al. | Tetraphenylborate-sensitive electrode for measuring membrane potential |