反应详情

温度

-78 °C

A 2 M solution of isopropyl magnesium chloride in tetrahydrofuran (65 μL, 0.13 mmol) is added to solution of 7-bromo-4-(2-pyridin-2-yl-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl)-quinoline (50.0 mg, 0.13 mmol) in tetrahydrofuran (1 mL) at room, temperature with stirring for 2 h. The mixture is cooled to −78° C. and triethylamine (21.4 μL, 0.154 mmol) and methanesulfonyl chloride (11 μL, 0.14 mmol) added. The mixture is warmed to room temperature and allowed to stand 18 h. The mixture is treated with water, extracted with ethyl acetate, dried (sodium sulfate), filtered, and concentrated in vacuo. The residue is chromatographed on SiO2 (dichloromethane to 75% ethyl acetate/dichloromethane) to yield the title compound as a solid, 4.5 mg (9%).

1. temperatureThe mixture is warmed to room temperature
2. waitto stand 18 h
3. extractionextracted with ethyl acetate
4. dry with materialdried (sodium sulfate)
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue is chromatographed on SiO2 (dichloromethane to 75% ethyl acetate/dichloromethane)