Reaktion #1182

ord-b9463e90fa6b413699ae9fcde2e663de

Reaktionsgleichung

[Cl][Sn][Cl]
SnCl2
O=N[O-].[Na+]
NaNO2
Nc1ccc(Cl)c(C(=O)O)c1
5-amino-2-chlorobenzoic acid
Cl.NNc1ccc(Cl)c(C(=O)O)c1
expected product
Ausbeute 123.1%
Cl.NNc1ccc(Cl)c(C(=O)O)c1
5-Hydrazino-2-chlorobenzoic acid hydrochloride
Ausbeute 123.1%

Lösungsmittel

Reaktionsbedingungen

Temperatur
-3°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled to -10° C.
  2. 2
    workup.STIRRINGThe mixture is stirred for one and a half hours at 0° C.
  3. 3
    Filtrationfiltered
  4. 4
    Sonstigethe precipitate is dried

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05723483uspto-grants-1998_03