反应详情

温度

105 °C

5-methyl-2-nitroaniline (1.0 g, 6.57 mmol), glycerol (1.88 g, 20.4 mmol), 3-nitrobenzenesulfonic acid sodium salt (1.92 g, 8.54 mmol) were added to H2SO4/H2O (6 ml, 7:5) solution and heated at 105° C. for 48 h. After completion of the reaction (monitored by LCMS), the mixture was cooled to 45° C. and poured slowly onto ice water (50 ml) and the mixture was extracted with DCM. The combined organic phases were dried (Na2SO4) and concentrated in vacuo to give the title compound (950 mg, 77%) which was used in the next step without purification.

1. customAfter completion of the reaction (monitored by LCMS)
2. temperaturethe mixture was cooled to 45° C.
3. additionpoured slowly onto ice water (50 ml)
4. extractionthe mixture was extracted with DCM
5. dry with materialThe combined organic phases were dried (Na2SO4)
6. concentrationconcentrated in vacuo