反应详情

To dimethylformamide (200 mL) add 4-nitrocatechol (13.8 g, 89 mmol), 4-methyl-N,N-bis[2-[[(4-methylphenyl)sulfonyl]oxy]ethyl]benzenesulfonamide (50.7 g, 89.4 mmol), and K2CO3 (27 g, 0.19 mol). Stir and heat the reaction at 110° C. Monitor the progress of the reaction by thin-layer chromatography. Upon completion remove the heat and add water (1.3 L) and methanol (300 mL). Collect the precipitate on paper by suction filtration. Wash the solid with water (2 L). Chromatograph the material on silica (300 g) with CH2Cl2 to obtain the title compound.

1. temperatureheat
2. customthe reaction at 110° C
3. customMonitor the progress of the reaction by thin-layer chromatography
4. customUpon completion remove the
5. temperatureheat
6. additionadd water (1.3 L) and methanol (300 mL)
7. customCollect the precipitate on paper
8. filtrationby suction filtration
9. washWash the solid with water (2 L)