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3-Hydroxybenzaldehyde → 3,3'-((2,2-Bis((3-formylphenoxy)methyl)propane-1,3-diyl)bis(oxy))dibenzaldehyde

HRID 1012367
ノート
印刷プレビュー

反応式

HRID 1012367 の反応式
[CH2:1](Br)[C:2]([CH2:7]Br)([CH2:5]Br)[CH2:3]Br.[OH:10][C:11]1[CH:12]=[C:13]([CH:16]=[CH:17][CH:18]=1)[CH:14]=[O:15].[C:19](=[O:22])([O-])[O-].[K+].[K+].[I-].[Na+]>O.CN(C)C=O>[CH:14]([C:13]1[CH:12]=[C:11]([CH:18]=[CH:17][CH:16]=1)[O:10][CH2:1][C:2]([CH2:7][O:10][C:11]1[CH:12]=[CH:13][CH:16]=[C:17]([CH:19]=[O:22])[CH:18]=1)([CH2:5][O:10][C:11]1[CH:18]=[CH:17][CH:16]=[C:13]([CH:14]=[O:15])[CH:12]=1)[CH2:3][O:10][C:11]1[CH:18]=[CH:17][CH:16]=[C:13]([CH:14]=[O:15])[CH:12]=1)=[O:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 1013-HydroxybenzaldehydeHCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 76701Propane, 1,3-dibromo-2,2-bis(bromomethyl)-

生成物 1

HCID 873530833,3'-((2,2-Bis((3-formylphenoxy)methyl)propane-1,3-diyl)bis(oxy))dibenzaldehyde収率 85.6%

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒

実験手順

5 g of pentaerythrityl tetrabromide, 9.5 g of 3-hydroxybenzaldehyde, 11 g of potassium carbonate, and a catalytic amount of sodium iodide were mixed. Thereto was added dimethylformamide, to conduct reaction at 130° C. for 6 hours. After cooled, water was added thereto, and the thus-precipitated crystal was collected by filtration. Dimethylformamide was added to this crystal, and the resultant solution was filtrated. Then, methanol was added to the filtrate, and the precipitated crystal was collected by filtration (yield amount 6.1 g, and yield 85.6%).

後処理

  1. customreaction at 130° C. for 6 hours
  2. temperatureAfter cooled
  3. filtrationthe thus-precipitated crystal was collected by filtration
  4. additionDimethylformamide was added to this crystal
  5. filtrationthe resultant solution was filtrated
  6. additionThen, methanol was added to the filtrate
  7. filtrationthe precipitated crystal was collected by filtration (yield amount 6.1 g, and yield 85.6%)

出典と根拠

ORDレコード
ord-85998706a5904299a8e8db1f112a5f31
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07977491B2

反応ノート

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