反应详情

The compound obtained in Step 1 (504 mg) was suspended in methylene chloride (20 ml) and to the suspension were added triethylamine (336 ml) and then 6-chloronaphthalene-2-sulfonyl chloride (600 mg) under cooling with ice. After stirring the mixture overnight at room temperature, saturated sodium chloride solution was added and the mixture was extracted with methylene chloride. The organic layer was dried over anhydrous sodium sulfate and thereafter the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent; n-hexane:ethyl acetate=20:1–4:1) to obtain the title compound (750 mg).

1. extractionthe mixture was extracted with methylene chloride
2. dry with materialThe organic layer was dried over anhydrous sodium sulfate
3. distillationthe solvent was distilled off under reduced pressure
4. customThe resulting residue was purified by silica gel column chromatography (eluent; n-hexane:ethyl acetate=20:1–4:1)