反应详情

1H-NMR (CDCl3) δ: 2.69 (3H, s), 3.85 (3H, s), 6.98 (2H, d, J=10 Hz), 7.50-7.80 (6H, m), 8.36 (1H) d) 7.8 g of 3-acetyl-2-[2-(4-methoxyphenyl)-vinyl]-5-benzofurancarbonitrile obtained in the above step c) was dissolved in a solvent mixture of 600 ml of tetrahydrofuran and 500 ml of ethanol. 900 mg of palladium oxide.1H2O.barium sulfate was added to the above solution, and the mixture was subjected to catalytic hydrogenation under normal pressure for 3.5 hours. After removing the catalyst by filtration, the resulting filtrate was concentrated to dryness. The residue thus obtained was extracted with ethyl acetate, and the resulting organic layer was washed with water, and dried to distill off the solvent. Thereafter, the residue thus obtained was washed with methanol to collect precipitated crystals by filtration, thereby obtaining 5.47 g of 3-acetyl-2-[2-(4-methoxyphenyl)ethyl]-5-benzofurancarbonitrile in the form of colorless prism crystals.

1. customobtained in the above step c)
2. customAfter removing the catalyst
3. filtrationby filtration
4. concentrationthe resulting filtrate was concentrated to dryness
5. customThe residue thus obtained
6. extractionwas extracted with ethyl acetate
7. washthe resulting organic layer was washed with water
8. customdried
9. distillationto distill off the solvent
10. customThereafter, the residue thus obtained
11. washwas washed with methanol
12. customto collect
13. customprecipitated crystals
14. filtrationby filtration