Methanol → HCID 66892336, compound

Temperature

100 °C

7-Iodo-5-nitro-1-benzofuran (2.5 g, 8.6 mmol) and iron (2.51 g, 45.0 mmol) were added to a round bottom flask. Methanol (25 mL), 1,4-dioxane (25 mL) and ammonium chloride (2.5 g, 46.7 mmol), dissolved in water (50 mL), were added and the mixture was heated at 100° C. for 16 h. The reaction mixture was filtered through Celite and volatiles were evaporated off. The residue was dissolved in a mixture of methanol (10 mL) and DCM (90 mL). This mixture was filtered through a silica plug and the solvent was evaporated yielding 2.22 g (99%) of the title compound as a brown oil. HPLC purity 70%, RT=1.26 min (System A; 10-97% MeCN over 3 min). MS (ESI+) for C8H6INO m/z is 260 (M+H)+.

1. additionwere added
2. filtrationThe reaction mixture was filtered through Celite and volatiles
3. customwere evaporated off
4. dissolutionThe residue was dissolved in a mixture of methanol (10 mL) and DCM (90 mL)
5. filtrationThis mixture was filtered through a silica plug
6. customthe solvent was evaporated

ORD record

ord-3b2b84cec6614fd187b8a111a0334f95

Source dataset

uspto-grants-2010_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07820675B2