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. is added m-chloroperoxybenzoic acid (2.75 g, 8.7 mmol). The reaction mixture is slowly warmed to 0° C. and then saturated NaHCO3 (10 ml) is added. The reaction mixture is partitioned between water (20 ml) and CH2Cl2 (20 ml), the layers are separated and then the aqueous layer is extracted with CH2Cl2 (20 ml). The CH2Cl2 extracts are combined, dried over MgSO4 and evaporated. The residue is 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 is partitioned between water (20 ml) and CH2Cl2 (20 ml)
2. customthe layers are separated
3. extractionthe aqueous layer is extracted with CH2Cl2 (20 ml)
4. dry with materialdried over MgSO4
5. customevaporated
6. customThe residue is purified by column chromatography on silica gel eluting with 50% ether/hexane