Hydrogen Peroxide → 1,2,3-Benzenetriol, 5-methyl-

HRID 1703405

반응식

HRID 1703405 반응식
[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

반응물 3

HCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 817442,6-Diformyl-4-methylphenol

생성물 1

HCID 5877901,2,3-Benzenetriol, 5-methyl-수율 69%

시약·촉매·용매 1

HCID 962Water용매2회

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

  1. customrose to 85° C.
  2. temperaturewas then maintained at 40°-50° C. with external cooling
  3. filtrationThe solution was filtered
  4. customto remove 1.05 parts
  5. 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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