反应详情

A mixture of 6-(1-Pyrenebutyryl)-3,10-bis(2-nitrobenzenesulfonyl)-3,6,10,16-tetraazabicyclo[10.3.1]-hexadeca-1(16),12,14-triene (2.26 g, 2.6 mmol), thiphenol (0.87 g, 7.8 mmol) and K2CO3 (3.22 g, 23.4 mmol) in 20 mL of DMF was stirred at rt overnight. The solvent was evaporated and the residue was dissolved in CHCl3—H2O. The organic phase was separated and the aqueous phase was extracted with CHCl3. The combined organic phase was dried (Na2SO4) and concentrated. The residue was purified by flash chromatography on a silica gel column using CH2Cl2 and then 3:1 CH2Cl2—MeOH as eluents to give 1.12 g (65%) of the title compound as a white foam.

1. customThe solvent was evaporated
2. dissolutionthe residue was dissolved in CHCl3—H2O
3. customThe organic phase was separated
4. extractionthe aqueous phase was extracted with CHCl3
5. dry with materialThe combined organic phase was dried (Na2SO4)
6. concentrationconcentrated
7. customThe residue was purified by flash chromatography on a silica gel column