反应详情

温度

0 °C

0.9 g (22.5 mmol) of a 60% suspension of sodium hydride in paraffin are added to a solution of 2.25 g (30.40 mmol) of tertbutanol in 27.5 ml of DMF. The whole is heated in a water bath for 30′ till the evolution of hydrogen ends. The system is cooled at 0° C. and 2.5 g (15.13 mmol) of ethyl 4-methylnicotinate in 2.5 ml of DMF are dropped with stirring. After 1.5 hr stirring at the same temperature, 3.4 g (18.37 mmol) of 4-bromobenzaldehyde in 2.5 ml DMF are dropped. The system is stirred at room temperature overnight. The solution is poured over 100 g of ice and is filtered. The filtrate is acidified with acetic acid and the solid is filtered, washed with water and dried, yielding 1.85 g (40%) of a product that is used directly in the next step.

1. additionare dropped
2. stirringThe system is stirred at room temperature overnight
3. filtrationis filtered
4. filtrationthe solid is filtered
5. washwashed with water
6. customdried