反应详情

A mixture of 29.6 g (95.7 mmol) of 7-benzyl-2-(trifluoromethyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-ol (prepared essentially as described in Step A, above) and 53 mL of phenylphosphonic dichloride in a 250-mL round bottom flask was heated at 150° C. After 2 h, the reaction was judged to be complete by TLC analysis. The mixture was cooled to ambient temperature and poured onto 400 g of ice, transferring with about 500 mL of ethyl acetate. The aqueous layer was neutralized with solid sodium bicarbonate and the layers separated. The aqueous layer was extracted with two portions of ethyl acetate. The combined organics were washed sequentially with saturated aqueous sodium bicarbonate solution and brine, dried over sodium sulfate and concentrated to give a brown solid. The solid was boiled in 2 L of hexane with charcoal, filtered, and concentrated in vacuo to give the title compound as a yellow solid. LC-MS 328 (M+1).

1. customprepared essentially
2. customthe layers separated
3. extractionThe aqueous layer was extracted with two portions of ethyl acetate
4. washThe combined organics were washed sequentially with saturated aqueous sodium bicarbonate solution and brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated
7. customto give a brown solid
8. filtrationfiltered
9. concentrationconcentrated in vacuo