反应 #1440789
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04351968
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Under a nitrogen atmosphere throughout: 5.3 Parts of 2-hydroxy-5-methylisophthalaldehyde prepared in Example 15 or 16 were slurried with a solution of 2.6 parts of sodium hydroxide in 32 parts of water, and a solution of 9.8 parts of 27.2% by weight hydrogen peroxide in 35 parts of water was added over four minutes. The temperature rose to 85° C. initially and was then maintained at 40°-50° C. with external cooling. After a further 18 minutes the pH was 7.8. The solution was filtered to remove 1.05 parts of unchanged starting material, and the filtrate was continuously extracted with ether to give 2.5 parts of 5-methylpyrogallol, m.pt. 114°-121° C., equivalent to 69% yield. rose to 85° C. was then maintained at 40°-50° C. with external cooling The solution was filtered to remove 1.05 parts the filtrate was continuously extracted with ether
来源 ID: ord-25d26f2d951f49f2ad2f279cbe6813ef