反应详情

温度

60 °C

3-Hydroxy-4-nitro-benzoic acid (10 g) was dissolved in MeOH (500 ml). 96% H2SO4 (2 ml) was added, and the mixture was heated to 60° C. for 18 hours. The reaction mixture was concentrated to approx. 200 ml, diluted with EtOAc (200 ml) and washed with an aqueous saturated solution of NaHCO3 (2×20 ml). The organic layer was dried over Na2SO4 and the solvent was removed by evaporation to yield 10.5 g of the desired intermediate.

1. concentrationThe reaction mixture was concentrated to approx. 200 ml
2. additiondiluted with EtOAc (200 ml)
3. washwashed with an aqueous saturated solution of NaHCO3 (2×20 ml)
4. dry with materialThe organic layer was dried over Na2SO4
5. customthe solvent was removed by evaporation