Reaktion #820688

Reaktionsgleichung

6-nitro-2,2-dimethyl-4H-1,3-benzodioxin-4-one

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title compound

Ausbeute 98.6%

6-amino-2,2-dimethyl-4H-1,3-benzodioxin-4-one

Ausbeute 98.6%

Lösungsmittel

EtOH

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe reaction mixture was filtered through a bed of celite
2. 2
   Waschenwashed with EtOH and THF
3. 3
   EinengenThe filtrates were concentrated under vacuum

Vorschrift

To a solution of 6-nitro-2,2-dimethyl-4H-1,3-benzodioxin-4-one (4.1 g) in EtOH (30 mL) was added Pd/C (1.947 g) under nitrogen atmosphere and then hydrogenated for 12 h at rt. The reaction mixture was filtered through a bed of celite, washed with EtOH and THF. The filtrates were concentrated under vacuum to give the title compound as pale yellow solid (3.5 g, 98%). 1H NMR (CDCl3) δ 7.71 (d, J=8.7 Hz, 1H), 7.15 (d, J=2.6 Hz, 1H), 6.83 (dd, J=8.7 Hz, 2.6 Hz, 1H), 3.44 (brs, 2H), 2.63 (s, 6H).

Quelle