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Hydrogen iodide → 2,3,6,7,10,11-Hexahydroxytriphenylene hydrate

HRID 2425743
ノート
印刷プレビュー

反応式

HRID 2425743 の反応式
C[O:2][C:3]1[C:20]([O:21]C)=[CH:19][C:18]2[C:17]3[C:12](=[CH:13][C:14]([O:25]C)=[C:15]([O:23]C)[CH:16]=3)[C:11]3[C:6](=[CH:7][C:8]([O:29]C)=[C:9]([O:27]C)[CH:10]=3)[C:5]=2[CH:4]=1.I>C(O)(=O)C>[OH2:2].[OH:2][C:3]1[C:20]([OH:21])=[CH:19][C:18]2[C:17]3[C:12](=[CH:13][C:14]([OH:25])=[C:15]([OH:23])[CH:16]=3)[C:11]3[C:6](=[CH:7][C:8]([OH:29])=[C:9]([OH:27])[CH:10]=3)[C:5]=2[CH:4]=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 2

HCID 24841Hydrogen iodideHCID 46073632,3,6,7,10,11-Hexamethoxytriphenylene

生成物 1

HCID 569245442,3,6,7,10,11-Hexahydroxytriphenylene hydrate収率 171.1%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Subsequently, to the obtained 2,3,6,7,10,11-hexamethoxytriphenylene (28.2 g, 0.069 moles), 57% hydroiodic acid (235.3 g, 1.05 moles) and acetic acid (145 mL) were added, and the solution was refluxed for 2 hours. After completion of the reaction, the solution was cooled down to room temperature, and the precipitated crystal was collected by filtration. The crystal collected by filtration was dried under reduced pressure to give gray type B crystal of 2,3,6,7,10,11-hexahydroxytriphenylene monohydrate (20.2 g, yield: 85.5%) (the method of JP-A-8-119894). Also, the resultant gray compound was confirmed to be 2,3,6,7,10,11-hexahydroxytriphenylene monohydrate by 1H-NMR analysis and measurement of water content by Karl-Fischer measuring instrument. In addition, the measurement results of X-ray powder diffraction spectrum of the type B crystal are shown in FIG. 5 and also, main peak values of the type B crystal are shown in Table 3. Also, the measurement of X-ray powder diffraction spectrum was carried out in the same way as in Example 6.

後処理

  1. temperaturethe solution was refluxed for 2 hours
  2. customAfter completion of the reaction
  3. filtrationthe precipitated crystal was collected by filtration
  4. filtrationThe crystal collected by filtration
  5. customwas dried under reduced pressure

出典と根拠

ORDレコード
ord-433a72342639418498c0ab091bcbbdb6
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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