反应详情

温度

80 °C

2-Fluoro-benzenesulfonyl chloride (0.11 mL, 0.81 mmol) was added to a solution of (4-Amino-7-isopropyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)-(2-amino-6-methyl-pyridin4-yl)-methanone (200 mg, 0.67 mmol) in pyridine (2 mL). The mixture was stirred for 2 h at 80° C. The reaction mixture was quenched with H2O (10 mL) and extracted with hot EtOAC/MeOH (95:5, 3×10 mL). The combined organic extracts were dried (Na2SO4), filtered, and concentrated in vacuo. Purification by flash column chromatography (ethyl acetate/MeOH 99:1) afforded the title compound as a yellow solid (91 mg, 30%). MS: 455.8 (MH+); HPLC Rf: 5.98 min. (HPLC method 4); HPLC purity: 100%.

1. customThe reaction mixture was quenched with H2O (10 mL)
2. extractionextracted with hot EtOAC/MeOH (95:5, 3×10 mL)
3. dry with materialThe combined organic extracts were dried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customPurification by flash column chromatography (ethyl acetate/MeOH 99:1)