Reaktion #2197613

Reaktionsgleichung

compound 422A

4-Bromo-7-nitrobenzofurazan

→

compound 422B

Ausbeute 95.1%

4-Bromo-7-aminobenzofurazan

Ausbeute 95.1%

Lösungsmittel

AcOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe resulting dark reaction mixture
2. 2
   Einengenconcentrated under reduced pressure
3. 3
   Waschenthe resulting solution was washed with sat. Na2CO3 solution
4. 4
   TrocknenThe organic layer was dried over Na2SO4
5. 5
   Einengenconcentrated in vacuo
6. 6
   Sonstigepurified by flash chromatography on silica gel eluting with 10-60% EtOAc in hexanes

Vorschrift

A solution of compound 422A (563 mg, 2.31 mmol) in AcOH (5 mL) was heated to 70° C. and Fe0 powder (258 mg, 4.62 mmol) was added in one portion. The resulting dark reaction mixture was stirred for 15 min, cooled to rt and concentrated under reduced pressure. The residue was taken up in EtOAc and the resulting solution was washed with sat. Na2CO3 solution. The organic layer was dried over Na2SO4, concentrated in vacuo and purified by flash chromatography on silica gel eluting with 10-60% EtOAc in hexanes to give 470 mg (95%) of compound 422B as a red solid.

Quelle