反应详情

Add 3-chlorobenzenecarboperoxoic acid (79.2 mg, 0.46 mmol) to a solution of 3-methylsulfanyl-5-phenylethynyl-pyridine, (prepared as described in EXAMPLE 128), (34.4 mg, 0.15 mmol) in dichloromethane (1 mL) at 0° C., warm to room temperature and stir for 2 h. Dilute with a 5% aqueous solution of sodium thiosulfite and dichloromethane. After separating the layers, sequentially wash the organic layer with a 5% aqueous solution of sodium thiosulfite and an aqueous saturated solution of sodium chloride, dry (magnesium sulfate), filter and concentrate. Purify the residue by silica gel chromatography, eluting with 100:0 to 100:50 hexanes:ethyl acetate, to give the title compound (24.8 mg, 64%).

1. customAfter separating the layers
2. washsequentially wash the organic layer with a 5% aqueous solution of sodium thiosulfite
3. dry with materialan aqueous saturated solution of sodium chloride, dry (magnesium sulfate)
4. filtrationfilter
5. concentrationconcentrate
6. customPurify the residue by silica gel chromatography
7. washeluting with 100:0 to 100:50 hexanes