反应详情

温度

-10 °C

4-(Cyclopropylcarbonyl)phenylacetonitrile, 15.5 g [JOC, 1973,16, 487] and methyl iodide, 15.5 ml, are dissolved in 75 ml THF. The mixture is cooled to −10° C. and a solution of potassium butoxide (24.5 g) in THF (75 ml) is added so that the temperature of the reaction is kept below 5° C. After 0.5 h more, HPLC shows the reaction to be complete. 200 ml 2M HCI is added followed by 200 ml toluene. The organics are washed with 100 ml 10%. sodium sulphite solution then 100 ml satd sodium chloride solution. The THF is removed and the toluene treated with 5 g silica to remove colour. The toluene is removed and the product crystallises. Yield, 19 g.

1. customis kept below 5° C
2. customthe reaction
3. addition200 ml 2M HCI is added
4. washThe organics are washed with 100 ml 10%
5. customThe THF is removed
6. additionthe toluene treated with 5 g silica
7. customto remove colour
8. customThe toluene is removed
9. customthe product crystallises
10. customYield