反应详情

To a stirred suspension of NaH (48 mg, 2 mmol) in dry NMP (2 mL) was added 2,4,6-trimethyl-benzene-1-thiol (191 mg, 1.2 mmol) The mixture was and stirred at room temperature for 30 min under argon. The reaction mixture was then added to a solution of 5-benzyl-4-chloro-5H-pyrrolo[3,2-d]pyrimidin-2-amine (103 mg, 0.4 mmol) in dry NMP (2.5 mL) and heated at 60° C. for 16 h. After completion of the reaction, the resulting mixture was diluted with water and washed with EtOAc. The combined organic layers were washed with water, 2% NaOH, and brine; dried over Na2SO4; filtered; and concentrated in vacuo. The crude product was purified by column chromatography, eluting with hexanes/ethyl acetate (2:1-1:3) to give the product as a light yellow solid (131 mg, 88%).

1. temperatureheated at 60° C. for 16 h
2. customAfter completion of the reaction
3. washwashed with EtOAc
4. washThe combined organic layers were washed with water, 2% NaOH, and brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationand concentrated in vacuo
8. customThe crude product was purified by column chromatography
9. washeluting with hexanes/ethyl acetate (2:1-1:3)