Hydrochloric Acid → 1,2,4-Benzotriazin-3-amine, 1-oxide

HRID 341788Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 341788
[N+:1]([C:4]1[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=1[NH2:6])([O-])=[O:2].[N:11]#[C:12][NH2:13].Cl.[OH-].[Na+]>C(O)(=O)C>[N+:1]1([O-:2])[C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=[C:12]([NH2:13])[N:11]=1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 69462-NitroanilineHCID 9864CyanamideHCID 14798Sodium Hydroxide

Produkt 1

HCID 794701,2,4-Benzotriazin-3-amine, 1-oxideAusbeute 78 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

A mixture of 10 g 2-nitroaniline and 20 g cyanamide is heated for 5 min to 100° C., cooled, mixed with 25 ml conc. hydrochloric acid and carefully heated to 70° C. After subsidence of the vigorous reaction, one cools to room temp., adds dropwise thereto 50 ml semiconce. caustic soda lye, heats for 30 min to 100° C., cools, filters and washes the precipitate with hot glacial acetic acid. There remain 9.1 g of title compound (78% of theory) of the m.p. 272°-274° C.

Aufarbeitung

  1. temperatureis heated for 5 min to 100° C.
  2. temperaturecooled
  3. customAfter subsidence of the vigorous reaction, one cools to room temp.
  4. additionadds dropwise

Quellen und Nachweise

ORD-Eintrag
ord-6afef906f78f490a9201b00e9d00908a
Quelldatensatz
uspto-grants-1999_01
Patentnummer
US05856325

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