反应详情

The mixture of potassium carbonate (158.7 mg, 1.15 mmol), compound 3 (100 mg, 0.38 mmol) and triethylene glycol (576 mg, 3.8 mmol) in anhydrous DMF (5.0 ml) was sealed in a microwavable vial (from Biotage) and subjected to microwave irradiation (Biotage Initiator system) at 180° C. for 25 min. After cooling to room temperature, water was added and reaction mixture was extracted with ethyl acetate. Organic layer was separated, washed with brine, dried over anhydrous sodium sulfate and evaporated. The residue was purified with PTLC (4% MeOH in DCM as developing solvent) gave product 7 (110 mg, Yield: 77%): 1H NMR (200 MHz, CDCl3): δ.8.20 (3H, m), 7.83 (1H, d, d, J1=8.6 Hz, J2=2.4 Hz), 7.61 (2H, d, J=8.8 Hz), 7.10 (2H, m) 6.84 (1H, d, J=8.6 Hz), 4.53 (2H, t, J=4.8 Hz), 3.88 (2H, t, J=4.8 Hz), 3.71 (6H, m), 3.61 (2H, m), 2.10 (1H, b), HRMS (EI) m/z calcd. for [C19H22N2O6]+ 374.1478.

1. customwas sealed in a microwavable vial (from Biotage)
2. customsubjected to microwave irradiation (Biotage Initiator system) at 180° C. for 25 min
3. customreaction mixture
4. extractionwas extracted with ethyl acetate
5. customOrganic layer was separated
6. washwashed with brine
7. dry with materialdried over anhydrous sodium sulfate
8. customevaporated
9. customThe residue was purified with PTLC (4% MeOH in DCM as developing solvent)