Methanol → Methyl 2-(2-iodophenyl)acetate

Temperatur

80 °C

2-(2-Iodophenyl)acetic acid (5.00 g, 19.1 mmol) was placed into a reaction flask and dissolved in MeOH (150 mL). Sulfuric acid (250 μL) was added and reaction mixture was stirred and heated at 80° C. under nitrogen for 16 hours. The resulting mixture was cooled to room temperature and the volatiles removed by evaporation under reduced pressure. The residue was taken up in ethyl acetate (100 mL), washed with 10% NaHCO3 (100 mL), dried (MgSO4) and evaporated under reduced pressure to give the title compound (I9) (5.20 g, 99%) as a clear liquid; 1H NMR (400 MHz, CDCl3) δ 7.85 (dd, J=7.9, 1.0 Hz, 1H), 7.35-7.27 (m, 2H), 6.97 (ddd, J=7.9, 7.0, 2.1 Hz, 1H), 3.81 (s, 2H), 3.72 (s, 3H).

1. customreaction mixture
2. temperatureThe resulting mixture was cooled to room temperature
3. customthe volatiles removed by evaporation under reduced pressure
4. washwashed with 10% NaHCO3 (100 mL)
5. dry with materialdried (MgSO4)
6. customevaporated under reduced pressure

ORD-Eintrag

ord-2cf4c02462914d50972e966902c90c66

Quelldatensatz

uspto-grants-2016_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09421205B2