反应详情

温度

0 °C

To a solution of 1-ethyl-4-chloro-6-(methylthio)-1H-pyrazolo[3, 4-b]quinoline (2.4 g, 8.7 mmol) in CHCl3 (50 mL) at -40° C. was added m-chloroperoxybenzoic acid (2.75 g, 8.7 mmol). The reaction mixture was slowly warmed to 0° C. and then saturated NaHCO3 (10 mL) was added. The reaction mixture was partitioned between water (20 mL) and CH2Cl2 (20 mL), the layers were separated and then the aqueous layer was extracted with CH2Cl2 (20 ml). The CH2Cl2 extracts were combined, dried over MgSO4 and evaporated. The residue was purified by column chromatography on silica gel eluting with 50% ether/hexane, then 25% ethyl acetate/25% hexane/50% ether and finally ethyl acetate (100%) to afford 2.4 g of 1-ethyl-4-chloro-6-(methylsulfinyl)-1H-pyrazolo[3,4-b]quinoline.

1. customThe reaction mixture was partitioned between water (20 mL) and CH2Cl2 (20 mL)
2. customthe layers were separated
3. extractionthe aqueous layer was extracted with CH2Cl2 (20 ml)
4. dry with materialdried over MgSO4
5. customevaporated
6. customThe residue was purified by column chromatography on silica gel eluting with 50% ether/hexane