反应 #3280565
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07005430B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of Compound 67a (240 mg, 0.585 mmol) obtained in Example 67 in tetrahydrofuran (2 mL) were added 2-methylthiopropanol (1 mL) and sodium hydride (containing 34% mineral oil, 88 mg, 2.34 mmol), then Compound 67a (240 mg, 0.585 mmol) was further added to the mixture, and stirring was continued at 100° C. for 4 hours. To the reaction mixture was added ethyl acetate, and the mixture was washed twice with water and dried over magnesium sulfate. The reaction mixture was concentrated, and the residue was purified by silica gel column chromatography (chloroform:methanol=99:1) to obtain the title compound (100 mg, 40%) as an ocher foamy solid. the mixture was washed twice with water dried over magnesium sulfate The reaction mixture was concentrated the residue was purified by silica gel column chromatography (chloroform:methanol=99:1)
来源 ID: ord-00725e3dbf5c496998a45d884879d53d