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Water → 4-[(4-Hydroxy-2,5-dimethylphenyl)methyl]benzene-1,3-diol

HRID 1625638
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HRID 1625638 반응식
[C:1]1([CH:8]=[CH:7][CH:6]=[C:4]([OH:5])[CH:3]=1)[OH:2].C1(C)C=CC(S(O)(=O)=O)=CC=1.O.O[CH2:22][C:23]1[C:24](CO)=[C:25]([CH3:31])[C:26]([OH:30])=[CH:27][C:28]=1[CH3:29]>C1(C)C=CC=CC=1.C(O)(=O)C>[OH:2][C:1]1[CH:8]=[CH:7][C:6]([CH2:22][C:23]2[CH:24]=[C:25]([CH3:31])[C:26]([OH:30])=[CH:27][C:28]=2[CH3:29])=[C:4]([OH:5])[CH:3]=1
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참가 물질

7

반응물 4

HCID 962WaterHCID 5054ResorcinolHCID 6101p-Toluenesulfonic acidHCID 86688865HCID 86688865, 화합물

생성물 1

HCID 225083514-[(4-Hydroxy-2,5-dimethylphenyl)methyl]benzene-1,3-diol수율 77.8%

시약·촉매·용매 2

HCID 176Acetic Acid용매
HCID 1140
Toluene
용매

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온도
25 °C

실험 절차

22.02 g of resorcinol, 1.90 g of p-toluene sulfonic acid, and 44.04 g of water are put in a 100 ml 4-necked flask, and 7.61 g of 4-hydroxymethyl(hydroxymethyl)-2,5-Xylenol is partly added thereto for one hour while maintaining at room temperature of 25° C. The mixture is reacted for 3 hours at the same temperature. Then, 50 g of acetic acid and 50 g of toluene are added to the reaction mass, separating a phase. The obtained organic layer is washed and concentrated. The obtained precipitate is filtered. The filtered product is rinsed with toluene, dried under reduced pressure for 24 hours, and treated through liquid chromatography, obtaining 7.94 g of 1,3-dihydroxy-4-(4-hydroxy-2,5-dimethyl benzyl)benzene having a purity of 99%.

후처리

  1. customThe mixture is reacted for 3 hours at the same temperature
  2. customseparating a phase
  3. washThe obtained organic layer is washed
  4. concentrationconcentrated
  5. filtrationThe obtained precipitate is filtered
  6. washThe filtered product is rinsed with toluene
  7. customdried under reduced pressure for 24 hours
  8. additiontreated through liquid chromatography

출처 및 근거

ORD 기록
ord-f1aaadce4d9248c8ad9bd6bbb8694c79
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08785103B2

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