反应详情

A solution of 6-(benzylthio)-1-(2-methoxy-4-(trifluoromethyl)phenyl)phthalazine 2 (0.340 g, 0.797 mmol) in 20 mL of MeCN, 0.75 mL of acetic acid, and 0.5 mL of water (20/0.75/0.5 ratio) was cooled to 0° C. and was treated with 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione (0.314 g, 1.595 mmol). After stirring for one hour, LC/MS showed mostly product, so the reaction mixture was diluted with DCM and was treated with MgSO4. After stirring for 10 minutes, the reaction mixture was filtered and concentrated. Purification of the crude residue by silica gel column chromatography (0 to 40% EtOAc/heptane) gave 1-(2-methoxy-4-(trifluoromethyl)phenyl)phthalazine-6-sulfonyl chloride (0.200 g, 0.497 mmol, 62.3% yield).

1. stirringAfter stirring for 10 minutes
2. filtrationthe reaction mixture was filtered
3. concentrationconcentrated
4. customPurification of the crude residue by silica gel column chromatography (0 to 40% EtOAc/heptane)