反应详情

温度

45 °C

Diphenyl ether (180 ml) was heated to about 230° C. (Internal temperature 200-210° C.) under inert atmosphere in a round bottom flask fitted with distillation set and a solution of diethyl ({[1-(4-methoxybenzyl)-1H-pyrazol-5-yl]amino}methylidene)propanedioate (85 gm, 0.227 mol) (example 2) in absolute ethanol (130 ml) was added dropwise. The reaction mixture was heated for about 2 hours. Volatile solubles were distilled out. The mixture was cooled to 45° C. and methanol (150 ml) was added dropwise. Solid, which precipitated out was filtered and washed with methanol and hexane and dried under vacuum.

1. customfitted with distillation
2. temperatureThe reaction mixture was heated for about 2 hours
3. distillationVolatile solubles were distilled out
4. additionmethanol (150 ml) was added dropwise
5. customSolid, which precipitated out
6. filtrationwas filtered
7. washwashed with methanol and hexane
8. customdried under vacuum