反应详情

A solution of the product of Example 2 (20 mg, 0.05 mmol) in dichloromethane (2 mL) containing Hunig's base (10 μL, 0.07 mmol) was treated with ethyl isocyanate (6 μL, 0.07 mmol) and stirred at room temperature for 8 hours. The mixture was diluted with water and extracted with dichloromethane. The aqueous layer was separated and extracted with additional dichloromethane, the organic layers were combined, dried over anhydrous magnesium sulphate, filtered and concentrated at reduced pressure. The residue was chromatographed on a Gilson HPLC to give the title compound (12 mg, 50%) as a yellow solid; MS(ES) m/e 444 [M+H]+.

1. extractionextracted with dichloromethane
2. customThe aqueous layer was separated
3. extractionextracted with additional dichloromethane
4. dry with materialdried over anhydrous magnesium sulphate
5. filtrationfiltered
6. concentrationconcentrated at reduced pressure
7. customThe residue was chromatographed on a Gilson HPLC