반응 #61076

반응 방정식

ammonium chloride

5-methyl-6-nitro-benzo(1,3)dioxole

ammonium chloride

→

title compound

수율 94.5%

6-Methyl-1,3-benzodioxol-5-amine

수율 94.5%

용매

MeOH H2O

반응 조건

후처리

1. 1
   여과Fe was filtered off
2. 2
   기타the solvent evaporated
3. 3
   기타The crude product was purified on an SCX cartridge (cHex/EtOAc 9:1)

실험 절차

A mixture of 5-methyl-6-nitro-benzo(1,3)dioxole (50 mg, 0.28 mmol), Fe (54 mg, 3.5 eq) and ammonium chloride (51.2 mg, 3.5 eq) in a 1:1 mixture of MeOH/H2O (2.8 mL) was subjected to microwave irradiation (60W, P=100 p.s.i.) at 80° C. for four 10 min periods. The brown solution was allowed to cool to r.t. and more Fe (3.5 eq) and ammonium chloride (3.5 eq) were added. The mixture was subjected to microwave irradiation (60W, P=100 p.s.i.) at 80° C. for an additional 10 min. Fe was filtered off and the solvent evaporated. The crude product was purified on an SCX cartridge (cHex/EtOAc 9:1) to give the title compound as a brown solid (40 mg, 93%).

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