Реакция #1528990

Уравнение реакции

compound 422A

4-Bromo-7-nitrobenzofurazan

→

compound 422B

Выход 95.1%

4-Bromo-7-aminobenzofurazan

Выход 95.1%

Растворители

AcOH

Условия реакции

Обработка

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

Методика

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.

Источник