Potassium Carbonate → 2,2-Dimethyl-6-nitro-2H-benzo[B][1,4]oxazin-3(4H)-one

Temperatur

70 °C

2-Amino-4-nitrophenol (5 g), ethyl 2-bromo-2-methylpropanoate (5.77 mL, 1.2 eq.), and K2CO3 (6.7 g, 1.5 eq.) were suspended in DMF (50 ml). The reaction mixture was heated at 70° C. overnight. The mixture was then diluted with water (200 mL) and EtOAc (150 mL). The EtOAc layer was washed with water (2×150 mL) and evaporated. The residue was purified by Combiflash chromatography (EtOAc in hexanes=10-100%) to give 2,2-dimethyl-6-nitro-2H-benzo[b][1,4]oxazin-3(4H)-one (3.45 g).

1. washThe EtOAc layer was washed with water (2×150 mL)
2. customevaporated
3. customThe residue was purified by Combiflash chromatography (EtOAc in hexanes=10-100%)

ORD-Eintrag

ord-df92a5e18c1642ca9ae5e98ad7e2710f

Quelldatensatz

uspto-grants-2016_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09321763B2