Reaktion #955505

Reaktionsgleichung

sodium fluoroborate

amino acid

2-(o-Aminophenylthio)-4-nitrobenzoic acid

sulfuric acid

sodium nitrite

→

2-(o-Hydroxyphenylthio)-4-nitrobenzoic acid

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturCool the mixture in an ice-bath
2. 2
   workup.STIRRINGstir for an additional 20 minutes
3. 3
   SonstigeSeparate the
4. 4
   Sonstigeprecipitated crude diazonium fluoroborate
5. 5
   Temperaturheat in an oil bath at 90°-100° C. for 45 minutes
6. 6
   TemperaturCool the mixture
7. 7
   Sonstigeseparate the precipitate

Vorschrift

Suspend 10.15 g (35 mmoles) of the amino acid of Step A in 75 ml of water and add 4 ml concentrated sulfuric acid (7.36 g, 75 mmoles, 140 meq.). Cool the mixture in an ice-bath and add 3.657 g (53 mmoles) of sodium nitrite in portions at 0°-5° C. Stir the suspension in the cold for 20 minutes. Add 10 g (91 mmoles) of sodium fluoroborate and stir for an additional 20 minutes. Separate the precipitated crude diazonium fluoroborate, suspend tne precipitate in 250 ml of 50% sulfuric acid and heat in an oil bath at 90°-100° C. for 45 minutes. Cool the mixture and separate the precipitate. (Yield: 7.76 g).

Quelle