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

HRID 1012367
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HRID 1012367 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6228Dimethylformamide용매

실험 절차

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%).

후처리

  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%)

출처 및 근거

ORD 기록
ord-85998706a5904299a8e8db1f112a5f31
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07977491B2

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