Reaktion #10494

Reaktionsgleichung

4-bromo-2-nitro-benzenethiol

disulfide

4-Bromo-2-nitro-benzenethiol

hydrogen

→

2-Amino-4-bromo-benzenethiol

Lösungsmittel

THF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationthe solids were filtered
2. 2
   FiltrationThe solid filter-cake
3. 3
   workup.DISSOLUTIONwas dissolved in pyridine (600 mL) at 100° C.
4. 4
   Filtrationfiltered
5. 5
   Sonstigeto remove the Ni residue

Vorschrift

The mixture of 4-bromo-2-nitro-benzenethiol and its disulfide from Example 2A (14.9 g, 53.5 mmol) in THF (450 mL) was mixed with Raney Ni (30 g, 100% wt). The mixture was hydrogenated in a 1000 mL Paar shaker at a hydrogen pressure of 40 psi at 50° C. for 41 hours. When the reaction was complete, the solids were filtered. The solid filter-cake was dissolved in pyridine (600 mL) at 100° C. and filtered to remove the Ni residue. This pyridine solution contained mostly the 2-amino-4-bromophenyldisulfide. Crude yield=11.9 g (92%)

Quelle