反应详情

To a mixture of 2-(3-fluoro-3′-hydroxybiphenyl-4-ylamino)nicotinic acid (1 g, 3.08 mmol) and NaHCO3 (0.5 g, 6.17 mmol) in acetone (20 ml) was added dropwise dimethyl sulphate (0.47 g, 3.70 mmol). The mixture was heated to reflux overnight and then concentrated. Ethyl acetate was added to the crude and washed twice with 4% solution of NaHCO3 and brine. The organic phase was then dried over MgSO4 and concentrated in vacuo to afford 0.4 g of solid beige pure enough for the next synthetic step. Yield=36%

1. temperatureThe mixture was heated
2. temperatureto reflux overnight
3. concentrationconcentrated
4. additionEthyl acetate was added to the crude
5. washwashed twice with 4% solution of NaHCO3 and brine
6. dry with materialThe organic phase was then dried over MgSO4
7. concentrationconcentrated in vacuo