[CH2:1]([CH:3]1[O:5][CH2:4]1)Cl.[OH:6][C:7]1[C:20]2[C:19](=[O:21])[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[S:12][C:11]=2[CH:10]=[C:9]([OH:22])[CH:8]=1.C([O-])([O-])=O.[K+].[K+]>CC(C)=O>[OH:6][C:7]1[C:20]2[C:19](=[O:21])[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[S:12][C:11]=2[CH:10]=[C:9]([O:22][CH2:1][CH:3]2[CH2:4][O:5]2)[CH:8]=1Epichlorohydrin (0.24 mL, 3.05 mmol) was added dropwise to a mixture of 1,3-dihydroxy-9H-thioxanthen-9-one (137 mg, 0.61 mmol) and K2CO3 (169 mg, 1.22 mmol) in anhydrous acetone (15 mL) in a dry round-bottom flask, followed by stirring under reflux at a temperature of 55 to 60° C. for one day. Solid of the reaction mixture was filtered and the solvent was removed under reduced pressure. The resulting residue was purified by silica gel column chromatography (developing solvent: CH2Cl2) to give the title compound (34 mg, 18.6%) as a yellow solid.
読み込み中…
