反应详情

温度

110 °C

10.0 g (37.7 mmol) of methyl 2-[1-amino-1-(4-fluorophenyl)methylene]-4-methyl-3-oxopentanoate were introduced into 50 ml of toluene together with 10.17 g (75.4 mmol) of N-cyano-N-methylmethanesulphonamide and the mixture was treated at room temperature with 3.61 g (18.9 mmol) of titanium tetrachloride. The reaction progressed exothermically. The red-orange-coloured suspension was heated to 110° C. and stirred for 4.5 h. It was then cooled to room temperature and treated with 30 ml of water. The organic phase was separated off and the aqueous phase was extracted with ethyl acetate (30 ml). The combined organic phases were washed with 30 ml of water and dried over magnesium sulphate. After filtering and concentrating the solution in a water-jet vacuum and drying in vacuo, 11.54 g of crude product were obtained in the form of a tacky oil.

1. temperatureIt was then cooled to room temperature
2. customThe organic phase was separated off
3. extractionthe aqueous phase was extracted with ethyl acetate (30 ml)
4. washThe combined organic phases were washed with 30 ml of water
5. dry with materialdried over magnesium sulphate
6. filtrationAfter filtering
7. concentrationconcentrating the solution in a water-jet vacuum
8. customdrying in vacuo