反应详情

To a solution of 7-amino-4-methyl-1H-quinolin-2-one (87 mg, 0.5 mmol) in dry DMF (2 ml) was added sodium hydride (24 mg, 60% disp. in oil, 0.6 mmol) followed by methyl iodide (38 μl, 0.6 mmol) and the reaction stirred at room temperature for 1.5 h. After quenching with water the mixture was extracted with EtOAc and the combined extracts were dried over MgSO4 and concentrated in vacuo to give the crude product. Purification by SPE column chromatography, eluting with 0-10% MeOH/EtOAc gradient gave title compound (64 mg) which was used in the next step without further purification. 1H NMR (250 MHz, CDCl3) δ (ppm): 7.47 (d, 1H), 6.59 (m, 2H), 6.55 (d, 1H), 4.45 (br, 2H), 3.61 (s, 3H), 2.38 (s, 3H).

1. customAfter quenching with water the mixture
2. extractionwas extracted with EtOAc
3. dry with materialthe combined extracts were dried over MgSO4
4. concentrationconcentrated in vacuo
5. customto give the crude product
6. customPurification by SPE column chromatography
7. washeluting with 0-10% MeOH/EtOAc gradient