反应 #3350565
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04053483
反应条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 38.2 g of pure phenol were mixed with 0.4 g of concentrated sulphuric acid, with stirring and heating to 60° C. 28.5 g (0.177 mole) of 7-methylisatin were added in portions. At the end of the addition, the temperature was raised to 85° C. and 21 g of PhOAc were gradually added dropwise over a period of 5 hours. Finally, the temperature of the stirred mixture was raised to 120° C. for 30 minutes. It was then allowed to cool, filtered and washed with abundant water to remove the PhOAc. The resulting solid was dried and gave 50 g. It was dissolved in acetone and precipitated with chloroform, allowed to cool and filtered. The solid formed was dried to yield 30 g of 3,3-bis-(4-hydroxyphenyl)-7-methyl-2 -indolinone, m.p. 272°-4° C. Yield: 52%. At the end of the addition the temperature was raised to 85° C. Finally, the temperature of the stirred mixture was raised to 120° C. for 30 minutes to cool filtered washed with abundant water to remove the PhOAc The resulting solid was dried gave 50 g precipitated with chloroform to cool filtered The solid formed was dried
来源 ID: ord-0c7136e6d5af4aee81d3e1c5a4576156