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

HRID 2425742
ノート
印刷プレビュー

反応式

HRID 2425742 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 7043Veratrole

生成物 2

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

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-e5838ccfc23044a2984831f8362c3628
出典データセット
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07964757B2

反応ノート

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