反应详情

A solution of Step 3 intermediate (13.5 g, 74.17 mmol) in dry DMF (148 ml) was added anhydrous K2CO3 (51.25 g, 370.85 mmol) and the mixture was stirred at room temperature for 1 h. Methyl iodide (34.74 g, 244.78 mmol) was added slowly with stirring and further stirred at room temperature for 24 h. The reaction mixture was diluted with water and the solid precipitated out was filtered, washed with water and dried to give 12.6 gm of the product as a brown solid; 1H NMR (300 MHz, DMSO-d6) δ 2.42 (s, 3H), 3.22 (s, 3H), 3.42 (s, 3H), 6.90 (s, 1H).

1. stirringwith stirring
2. stirringfurther stirred at room temperature for 24 h
3. customthe solid precipitated out
4. filtrationwas filtered
5. washwashed with water
6. customdried