反应详情

温度

60 °C

To a solution of tert-butyl (2-nitro-4-(thiophen-2-yl)phenyl)carbamate (1.6 g, 4.99 mmol, 1 eq.) in methanol (20 mL) was added hydrazine hydrate (14 mL) and ferric chloride (0.05 g, 0.3 mmol, 0.06 eq.). The resulting mixture was warmed to 60° C. and stirred for 2 h. The reaction was then filtered through Celite, the solids were washed with MeOH. The filtrate was concentrated under reduced pressure. Water was added to the residue and the suspension was stirred for 1 h. The obtained solid was filtered, washed with hexanes then dried to yield tert-butyl (2-amino-4-(thiophen-2-yl)phenyl)carbamate (1.2 g, 83% yield).

1. filtrationThe reaction was then filtered through Celite
2. washthe solids were washed with MeOH
3. concentrationThe filtrate was concentrated under reduced pressure
4. additionWater was added to the residue
5. stirringthe suspension was stirred for 1 h
6. filtrationThe obtained solid was filtered
7. washwashed with hexanes
8. customthen dried