反应详情

温度

0 °C

A suspension of sodium hydride (4.87 g, 121.7 mmole) in 18 mL dry DMF was cooled to 0° C. and then 5-nitrovanillin (20 g, 101.4 mmole) in 30 mL of DMF was added dropwise. After 30 minutes, methyl iodide (43.18 g, 304.2 mmole) was added dropwise at 0° C. When the addition was completed, the mixture was warmed to room temperature and stirred overnight. Water was added and the solution extracted with ethyl ether, the organic layer was washed with 10% NaOH solution, dried over MgSO4, filtered and evaporated in vacuo to an oil (8.7 g, 40.7%).

1. additionWhen the addition
2. temperaturethe mixture was warmed to room temperature
3. extractionthe solution extracted with ethyl ether
4. washthe organic layer was washed with 10% NaOH solution
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customevaporated in vacuo to an oil (8.7 g, 40.7%)