反应 #3497475
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US05081121
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Two grams of 2-benzyloxy-3-methoxyaniline and 2.3 g of diethyl ethoxymethylenemalonate were heated at a temperature of 100°-120° C. for 1 hour. Fifty milliliter of diphenyl ether was added to the mixture, and the resulting mixture was further heated at 250°-270° C. for 1.5 hours. After the mixture was cooled down to room temperature, it was purified by silica gel column chromatography (Wako Gel C-200, 100 g). Elution with a mixed solvent of chloroform (95 parts) and methanol (5 parts) gave 980 mg of 3-ethoxycarbonyl-8-hydroxy-7-methoxy-4(1H)-quinolone. the resulting mixture was further heated at 250°-270° C. for 1.5 hours it was purified by silica gel column chromatography (Wako Gel C-200, 100 g) Elution with a mixed solvent of chloroform (95 parts) and methanol (5 parts)
来源 ID: ord-ef8294e4d00340069049079b77a40ccc