Hydrogen Peroxide → 1,2,3-Benzenetriol, 5-methyl-
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[OH:1][C:2]1[C:9](C=O)=[CH:8][C:7]([CH3:12])=[CH:6][C:3]=1C=O.[OH-:13].[Na+].[OH:15]O>O>[CH3:12][C:7]1[CH:6]=[C:3]([OH:15])[C:2]([OH:1])=[C:9]([CH:8]=1)[OH:13]참가 물질
5
실험 절차
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.
후처리
- customrose to 85° C.
- temperaturewas then maintained at 40°-50° C. with external cooling
- filtrationThe solution was filtered
- customto remove 1.05 parts
- extractionthe filtrate was continuously extracted with ether
출처 및 근거
- ORD 기록
- ord-25d26f2d951f49f2ad2f279cbe6813ef
- 출처 데이터셋
- uspto-grants-1982_09
- 특허 번호
- US04351968
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