Stannous Chloride → 2,3-Dimethyl-4-hydrazinobenzoic acid hydrochloride

HRID 1083

Reaktionsgleichung

Reaktionsgleichung von HRID 1083
[N:1]([O-])=O.[Na+].[NH2:5][C:6]1[CH:14]=[CH:13][C:9]([C:10]([OH:12])=[O:11])=[C:8]([CH3:15])[C:7]=1[CH3:16].[Cl:17][Sn]Cl>O.Cl>[ClH:17].[CH3:15][C:8]1[C:7]([CH3:16])=[C:6]([NH:5][NH2:1])[CH:14]=[CH:13][C:9]=1[C:10]([OH:12])=[O:11]

Komponenten

6

Edukt 3

HCID 24479Stannous ChlorideHCID 27627774-Amino-2,3-dimethylbenzoic acidHCID 23668193Sodium Nitrite

Produkt 1

HCID 702445822,3-Dimethyl-4-hydrazinobenzoic acid hydrochlorideAusbeute 93,7 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittel2×HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
-5 °C

Versuchsvorschrift

A solution of 1.87 g of NaNO2 in 7 ml of water is added slowly to a solution, cooled to -5° C., of 4.5 g of 4-amino-2,3-dimethylbenzoic acid in 135 ml of concentrated HCl. After 2 hours of stirring at -5° C., a solution of 25 g of SnCl2 ·2H2O in 250 ml of concentrated HCl is added at -10° C., and the mixture is stirred for 30 minutes at -5° C. and then 2 hours at RT. The mixture is filtered, and the precipitate is washed with 5 ml of concentrated HCl and dried under a stream of dry nitrogen and then under vacuum to obtain 5.5 g of expected product.

Aufarbeitung

  1. stirringthe mixture is stirred for 30 minutes at -5° C.
  2. custom2 hours
  3. customat RT
  4. filtrationThe mixture is filtered
  5. washthe precipitate is washed with 5 ml of concentrated HCl
  6. customdried under a stream of dry nitrogen

Quellen und Nachweise

ORD-Eintrag
ord-70a25d6a367f495c9c26f59a04ae0cc2
Quelldatensatz
uspto-grants-1998_03
Patentnummer
US05723483

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