5-Amino-2-chlorobenzoic acid → 2-Chloro-5-hydrazinylbenzoic acid hydrochloride

HRID 582769

Reaktionsgleichung

Reaktionsgleichung von HRID 582769
[N:1]([O-])=O.[Na+].[NH2:5][C:6]1[CH:7]=[CH:8][C:9]([Cl:15])=[C:10]([CH:14]=1)[C:11]([OH:13])=[O:12].O.O.Cl[Sn]Cl>O.Cl>[ClH:15].[NH:5]([C:6]1[CH:7]=[CH:8][C:9]([Cl:15])=[C:10]([CH:14]=1)[C:11]([OH:13])=[O:12])[NH2:1]

Komponenten

6

Edukt 3

HCID 378795-Amino-2-chlorobenzoic acidHCID 61436Stannous chloride dihydrateHCID 23668193Sodium Nitrite

Produkt 1

HCID 164957252-Chloro-5-hydrazinylbenzoic acid hydrochlorideAusbeute 123,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidLösungsmittel2×HCID 962WaterLösungsmittel2×

Reaktionsbedingungen

Temperatur
-3 °C

Versuchsvorschrift

A solution of 2.11 g of NaNO2 in 40 ml of water is added over 30 minutes to a suspension, cooled to -2° C., of 5 g of 5-amino-2-chlorobenzoic acid in 50 ml of concentrated HCl. The solution is stirred for 2 hours at -3° C. and cooled to -10° C., and a solution of 23 g of SnCl2.2H2O in 20 ml of concentrated HCl and 20 ml of water is added over 30 minutes. The mixture is stirred for one and a half hours at 0° C. and filtered, and the precipitate is dried to obtain 4 g of expected product.

Aufarbeitung

  1. temperaturecooled to -10° C.
  2. stirringThe mixture is stirred for one and a half hours at 0° C.
  3. filtrationfiltered
  4. customthe precipitate is dried

Quellen und Nachweise

ORD-Eintrag
ord-6ca3a4300596418a926de5c4fa29c061
Quelldatensatz
uspto-grants-1999_07
Patentnummer
US05925661

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