反应详情

温度

65 °C

48% hydrobromic acid (3.0 mL) was added to a solution of (5R)-5-[(E)-2-(5-acetyl-6-methoxypyridin-2-yl)-2-(4-tert-butylphenyl)ethenyl]-1-(2,4-dimethoxybenzyl)pyrrolidin-2-one (300 mg) in 1,4-dioxane (3.0 mL), and the mixture was stirred at 65° C. for 0.5 hour. Water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate, after which the solvent was evaporated under reduced pressure. Anisole (2 mL) was added to a solution of the residue (278 mg) in trifluoroacetic acid (1 mL), and the mixture was stirred at 80° C. for 4.5 hours. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform:methanol=1:0→9:1) to give the title compound as a yellow powder (103 mg).

1. extractionfollowed by extraction with ethyl acetate
2. washThe organic layer was washed with brine
3. dry with materialdried over anhydrous magnesium sulfate
4. customafter which the solvent was evaporated under reduced pressure
5. additionAnisole (2 mL) was added to a solution of the residue (278 mg) in trifluoroacetic acid (1 mL)
6. stirringthe mixture was stirred at 80° C. for 4.5 hours
7. customThe solvent was evaporated under reduced pressure
8. customThe residue was purified by silica gel column chromatography (chloroform:methanol=1:0→9:1)