反应详情

To a solution of 2-(2-hydroxyethyl)-3-hydroxymethyl-5-pyridin-2-yl-4-quinoline-4-yl-pyrazole, (0.10 g, 0.29 mmol) in tetrahydrofuran (10 mL) cooled at 0° C. is added NaH (0.04 g, 50% in mineral oil). The mixture is stirred for 2 h at room temperature and methanesulfonyl chloride (0.065 g, 0.57 mmol) is added dropwise over 30 min. The reaction is quenched with water and extracted into ethyl acetate. The organic layer is washed with water, dried (sodium sulfate), filtered, and concentrated in vacuo. The residue is chromatographed on SiO2 (10% methanol/dichloromethane) to yield the title compound, 31 mg (33%), as a white solid.

1. customThe reaction is quenched with water
2. extractionextracted into ethyl acetate
3. washThe organic layer is washed with water
4. dry with materialdried (sodium sulfate)
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue is chromatographed on SiO2 (10% methanol/dichloromethane)