反应详情

温度

80 °C

Potassium carbonate (60.4 g, 437 mmol) and iodoethane (17.6 mL, 218.4 mmol) were added to a mechanically stirred solution of 2-hydroxy-4-nitro-benzoic acid (10.0 g, 54.6 mmol) in 2-butanone (165 mL). The resulting mixture was heated in an 80° C. oil bath for 16 h and then allowed to cool. TLC (20% ethyl acetate in hexanes) showed consumption of starting material. The reaction mixture was concentrated to dryness, and the residue was taken up in ethyl acetate and washed three times with a saturated solution of sodium thiosulfate, dried over magnesium sulfate and concentrated to give ethyl 2-ethoxy-4-nitro-benzoate as a yellow solid (12.7 g, 97%). LC-MS: 240.1 [(M+H)+].

1. temperatureto cool
2. customconsumption of starting material
3. concentrationThe reaction mixture was concentrated to dryness
4. washwashed three times with a saturated solution of sodium thiosulfate
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated