反应详情

Sodium iodide (720 mg, 4.8 mmol) and hydriodic acid (2.0 mL, 47% aqueous solution) were added to the solution of 7-benzyl-4-chloro-5,6,7,8-tetrahydro-2-(methoxymethyl)pyrido[3,4-d]pyrimidine as prepared for Example 5.B. and (1.2 g, 4.0 mmol) and 4-aminobenzotrifluoride (1.3 g, 8 mmol) in dioxane (20 mL) and the reaction solution was stirred at 100° C. overnight. Solvent was removed in vacuo and the residue was dissolved in water. Solid sodium carbonate was added to the solution to a pH>7 then extracted by ethyl acetate. Ethyl acetate phase was washed by brine, and dried over sodium sulfate. Solvent was removed and the residue was purified by column chromatography to yield the product as a beige solid (910 mg, 54%).

1. customas prepared for Example 5.B
2. customSolvent was removed in vacuo
3. dissolutionthe residue was dissolved in water
4. additionSolid sodium carbonate was added to the solution to a pH>7
5. extractionthen extracted by ethyl acetate
6. washEthyl acetate phase was washed by brine
7. dry with materialdried over sodium sulfate
8. customSolvent was removed
9. customthe residue was purified by column chromatography