反应详情

A mixture of the product from step (c) (8.9 g). dimethyl acetylmethylphosphonate (6.84 g), anhy. potassium carbonate (11.37 g) and dry THF (100 ml) was heated under N2 at 50°-55° C. for 20 hours. The mixture was then cooled and filtered, the residue washed with THF, and the filtrate and washings combined and stripped to give a pale orange oil which was eluted through a silica gel column using ether/40-60 pet. ether (1:2) and the eluate stripped and dried under high vacuum to give the desired product as a very pale yellow, viscous oil (5.59 g).

1. temperatureThe mixture was then cooled
2. filtrationfiltered
3. washthe residue washed with THF
4. customto give a pale orange oil which
5. washwas eluted through a silica gel column
6. customdried under high vacuum