反应详情

温度

-75 °C

2-Picoline (2 g) was dissolved in tetrahydrofuran (30 ml) and the solution was cooled to −75° C. Butyl lithium (14.73 ml. of a 1.6M-solution in hexane) was added dropwise and the mixture stirred for 2 h. Dimethylacetamide (1.87 ml) was then added dropwise and the reaction was allowed to warm up to room temperature and stirring was continued for a further 2 h. Water (8.6 ml) and 36% hydrochloric acid (1.3 ml) were added and after stirring for another 30 minutes, ethyl acetate was added. The separated solvent phase was washed with brine and then dried (MgSO4). On evaporation an oil was obtained and used without further purification.

1. temperatureto warm up to room temperature
2. stirringstirring
3. waitwas continued for a further 2 h
4. stirringafter stirring for another 30 minutes
5. washThe separated solvent phase was washed with brine
6. dry with materialdried (MgSO4)
7. customOn evaporation an oil
8. customwas obtained
9. customused without further purification