反应详情

1.0 mL of triethylamine was added under ice cooling to a 15 mL chloroform solution of 1.02 g of 3,5-dichloro-3-(2-methoxyphenyl)-1,3-dihydro-2H-indol-2-one and 530 mg of the compound obtained in step 8-2, after which the reaction mixture was stirred for 18.5 hours at room temperature. 20 mL of a 5% potassium carbonate aqueous solution was poured into the reaction solution under stirring, and extraction was performed with chloroform (20 mL×2). The combined organic layer was washed with saturated brine and dried with sodium sulfate, then the drying agent was filtered off and the solvent was distilled off under reduced pressure. The residue thus obtained was separated and purified by column chromatography (silica gel 60, mobile phase: ethyl acetate/acetone=98/2; v/v) to obtain two kinds of diastereoisomer of the titled compound in amounts of 708 mg (isomer A: colorless, amorphous) and 501 mg (isomer B: colorless, amorphous).

1. stirringunder stirring
2. extractionextraction
3. washThe combined organic layer was washed with saturated brine
4. dry with materialdried with sodium sulfate
5. filtrationthe drying agent was filtered off
6. distillationthe solvent was distilled off under reduced pressure
7. customThe residue thus obtained
8. customwas separated
9. custompurified by column chromatography (silica gel 60, mobile phase: ethyl acetate/acetone=98/2; v/v)