反应详情

A mixture of 1-pyrenebutyric acid (0.87 g, 3.0 mmol) and 4-methylmorpholine (0.59 g, 5.9 mmol) in 20 mL of anhydrous CH2Cl2 was stirred at rt for 30 min. After addition of 1,3-dicyclohexylcarbodiimide (DCC) (0.62 g, 3.0 mmol) and 1-hydroxybenzotriazole (HOBT) (0.41 g, 3.0 mmol), the resulting solution was stirred at rt for another 30 min. A solution of 3,10-bis(2-nitrobenzenesulfonyl)-3,6,10,16-tetraazabicyclo[10.3.1]hexadeca-1(16),12,14-triene (from Example 72, 1.77 g, 3.0 mmol) was added to the above solution and the resulting solution was stirred at rt for 40 h. The solution was filtered and the filtrate was washed with brine , dried (Na2SO4) and concentrated. The residue was purified by flash chromatography on a silica gel column using 100:1 CH2Cl2—MeOH as an eluent to give 2.36 g (92%) of the title compound as a pale yellow foam.

1. stirringthe resulting solution was stirred at rt for another 30 min
2. stirringthe resulting solution was stirred at rt for 40 h
3. filtrationThe solution was filtered
4. washthe filtrate was washed with brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. customThe residue was purified by flash chromatography on a silica gel column