反应详情

温度

15 °C

To a mixture of 54 g of the compound of Example 2 in 200 mL of chloroform (ethanol-free) and of N,N-dimethylaniline, a solution of 30 g of thionyl chloride in 50 mL of chloroform (ethanol-free) was added while maintaining the reaction temperature at 15° C. with an ice-water bath. The mixture was stirred at 25° C. for 1 hour, then refluxed for 3 hours. The mixture was acidified with 1 N aqueous hydrochloric acid and the organic layer was collected. The organic layer was washed once with 1 N aqueous hydrochloric acid, dried over magnesium sulfate, and filtered. The filtrate was passed through a silica gel column, eluted with methylene chloride, and after evaporation of the eluant, 54 g subject compound was obtained as a yellow oil.

1. temperaturerefluxed for 3 hours
2. customthe organic layer was collected
3. washThe organic layer was washed once with 1 N aqueous hydrochloric acid
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. washeluted with methylene chloride
7. customafter evaporation of the eluant, 54 g
8. customwas obtained as a yellow oil