反应详情

温度

60 °C

m-CPBA (148 mg, 0.6 mmol) was added to a solution of N-(4-tert-butylphenyl)-7-(3-chloropyridin-2-yl)-5,6,7,8-tetrahydro-2-(methylthio)pyrido[3,4-d]pyrimidin-4-amine from Example 28.C. (88 mg, 0.2 mmol) in ethanol (7 mL) and stirred at room temperature for 1 hr. Solid thus formed was filtered out and dried in vacuo (50 mg). The solid was suspended in methanol (5 mL) and sodium methoxide (9 mg, 0.165 mmol) was added and stirred at 60° C. overnight. Solvent was removed in vacuo and residue was dissolved in ethyl acetate, washed with water, sodium hydrosulfite aqueous solution, brine and dried over sodium sulfate. Purified by flash chromatography to yield the product as a white solid (33 mg).

1. customSolid thus formed
2. filtrationwas filtered out
3. customdried in vacuo (50 mg)
4. customSolvent was removed in vacuo and residue
5. dissolutionwas dissolved in ethyl acetate
6. washwashed with water, sodium hydrosulfite aqueous solution, brine
7. dry with materialdried over sodium sulfate
8. customPurified by flash chromatography