反応 #2121511
関連文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08691816B2
反応条件: temp:45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: Sodium methoxide (in portions) was added, over a time interval of about three minutes, to 4-acetyl-benzamide (1.38 g, 8.5 mmol) and 5-methoxy-furan-2-carbaldehyde (1.31 g, 10.6 mmol) in a 1:1 mixture of methanol and dimethylformamide (16 mL). The resulting solution was placed under N2 and stirred overnight at 45° C. The reaction mixture was then evaporated to dryness under vacuum, followed by the addition of water and brine (100 mL) to the resulting residue. The aqueous solution was extracted with ethyl acetate (125 mL×3) and the combined organic layers were washed with brine (100 mL) and dried over MgSO4. The crude reaction mixture of 4-[(E)-3-(5-methoxy-furan-2-yl)-acryloyl]-benzamide and unreacted 4-acetyl acetamide is used without purification. The reaction mixture was then evaporated to dryness under vacuum followed by the addition of water and brine (100 mL) to the resulting residue The aqueous solution was extracted with ethyl acetate (125 mL×3) the combined organic layers were washed with brine (100 mL) dried over MgSO4 The crude reaction mixture of 4-[(E)-3-(5-methoxy-furan-2-yl)-acryloyl]-benzamide and unreacted 4-acetyl acetamide is used without purification
ソース ID: ord-1f816030681246f4ad5bc4ba5f7cd4e2