Sulfamic Acid → HCID 54018568, Verbindung

HRID 258796

Reaktionsgleichung

Reaktionsgleichung von HRID 258796
[Cl:1][C:2]1[CH:8]=[CH:7][C:6]([Cl:9])=[CH:5][C:3]=1[NH2:4].N([O-])=O.[Na+].S(=O)(=O)(O)N.[NH+:19]([O-])=O.[CH3:22][CH2:23][O:24][CH2:25][CH2:26][O:27][CH2:28][CH2:29][N:30]([CH2:37][CH3:38])[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1.C([O-])(=O)C.[Na+]>Cl.O>[Cl:1][C:2]1[CH:8]=[CH:7][C:6]([Cl:9])=[CH:5][C:3]=1[N:4]=[N:19][C:34]1[CH:33]=[CH:32][C:31]([N:30]([CH2:29][CH2:28][O:27][CH2:26][CH2:25][O:24][CH2:23][CH3:22])[CH2:37][CH3:38])=[CH:36][CH:35]=1

Komponenten

9

Edukt 6

HCID 5987Sulfamic AcidHCID 72622,5-DichloroanilineHCID 517045Sodium AcetateHCID 21424342N-[beta-(beta-ethoxy)ethoxy]ethyl-N-ethylanilineHCID 23668193Sodium NitriteHCID 178526385HCID 178526385, Verbindung

Produkt 1

HCID 54018568HCID 54018568, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittel2×HCID 962WaterLösungsmittel3×

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

16.1 g (0.1 mole) of 2,5-dichloroaniline was dissolved in a mixed solution of 85 ml of concentrated hydrochloric acid and 200 ml of water while stirring with heating on a water bath and the solution was cooled to 5° C and a solution prepared by dissolving 8.28 g (0.12 mole) of sodium nitrite in 50 ml of water was slowly added dropwise. The temperature was kept at 5° C and after completion of the addition of the solution was stirred for 20 minutes, sulfamic acid was added thereto to decompose excess HNO2. Thereafter, the solution was filtered and added at a time to a solution prepared by dissolving 23.6 g (0.1 mole) of N-[β-(β-ethoxy)ethoxy]ethyl-N-ethylaniline in 1 l of 1N-HCl. Furthermore, about 500 ml of water was added thereto and with stirring about 200 g of sodium acetate were added thereto. After allowing to stand for several hours, it was filtered and the azo dye which adhered to wall of device and filter paper was collected and used for the next reaction without purification. The crude product was 34.1 g.

Aufarbeitung

  1. temperaturewith heating on a water bath
  2. customa solution prepared
  3. additionwas slowly added dropwise
  4. customwas kept at 5° C
  5. additionafter completion of the addition of the solution
  6. stirringwas stirred for 20 minutes
  7. filtrationThereafter, the solution was filtered
  8. additionadded at a time to a solution
  9. customprepared
  10. additionwere added
  11. waitto stand for several hours
  12. filtrationit was filtered
  13. filtrationfilter paper
  14. customwas collected
  15. customused for the next reaction without purification

Quellen und Nachweise

ORD-Eintrag
ord-1710c168a65e4362bac6e98310e89f7b
Quelldatensatz
uspto-grants-1977_07
Patentnummer
US04035188

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