Reaktion #3354

Reaktionsgleichung

NaOH

2,2'-Dithiobis(5-nitrobenzamide)

acetic acid

→

2,2'-Dithiobis(5-aminobenzamide)

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe resulting slurry was heated
2. 2
   Temperaturat reflux for 2.0 hours
3. 3
   FiltrationThe alkaline mixture was filtered
4. 4
   workup.ADDITIONacetic acid was added to the solution
5. 5
   SonstigeWhile bubbling oxygen into the solution
6. 6
   Temperatura pH=6-7 was maintained with the addition of acetic acid
7. 7
   SonstigeA solid gradually formed as the pH
8. 8
   FiltrationThe product (1.1 g) was recovered by filtration, mp 188°-190° C.

Vorschrift

2,2'-Dithiobis(5-nitrobenzamide) (2.6 g, 7.0 mmol) was added portion-wise to a refluxing slurry of reduced iron (8.7 g) in 65 mL of water containing 0.1 mL of acetic acid. The resulting slurry was heated at reflux for 2.0 hours, then cooled to room temperature. The slurry was made strongly basic (pH 11) by the addition of 14 mL of 1N NaOH. The alkaline mixture was filtered, and acetic acid was added to the solution to adjust the pH to 7.0. While bubbling oxygen into the solution, a pH=6-7 was maintained with the addition of acetic acid. A solid gradually formed as the pH begins to stabilize. The product (1.1 g) was recovered by filtration, mp 188°-190° C.

Quelle