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Veratrole → 2,3,6,7,10,11-Hexamethoxytriphenylene

HRID 1925789
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HRID 1925789 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[O:9][CH3:10]>S(=O)(=O)(O)O>[OH2:2].[OH:9][C:4]1[C:3]([OH:2])=[CH:8][C:7]2[C:6]3[C:5](=[CH:4][C:3]([OH:2])=[C:8]([OH:2])[CH:7]=3)[C:6]3[C:7](=[CH:8][C:3]([OH:2])=[C:4]([OH:9])[CH:5]=3)[C:6]=2[CH:5]=1.[CH3:1][O:2][C:3]1[C:4]([O:9][CH3:10])=[CH:5][C:6]2[C:7]3[C:6](=[CH:5][C:4]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:8]=3)[C:7]3[C:6](=[CH:5][C:4]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:8]=3)[C:7]=2[CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 7043Veratrole

생성물 2

HCID 46073632,3,6,7,10,11-Hexamethoxytriphenylene수율 240.1%HCID 569245442,3,6,7,10,11-Hexahydroxytriphenylene hydrate

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

A type B crystal of 2,3,6,7,10,11-hexahydroxytriphenylene monohydrate was synthesized according to the process described in Synthesis, 477, 1994 and JP-A-8-119894. Namely, 1,2-dimethoxybenzene (31.78 g, 0.23 moles) and anhydrous ferric chloride (120 g, 0.74 moles) were dissolved in 70% sulfuric acid, and the solution was reacted at 25° C. for 24 hours with stirring. After completion of the reaction, the solution was poured into ice water (500 g), and the precipitated crystal was collected by filtration. After the resultant crystal was washed with water (1 L), and then dried to give pale purple colored 2,3,6,7,10,11-hexamethoxytriphenylene (28.2 g, theoretical yield from 1,2-dimethoxybenzene: 90.1%) (the method of Synthesis, 477, 1994).

후처리

  1. customdescribed in Synthesis, 477, 1994 and JP-A-8-119894
  2. customthe solution was reacted at 25° C. for 24 hours
  3. customAfter completion of the reaction
  4. filtrationthe precipitated crystal was collected by filtration
  5. washAfter the resultant crystal was washed with water (1 L)
  6. customdried

출처 및 근거

ORD 기록
ord-fb1c824139514220ae6415ee0d38c5f3
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08178731B2

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