Water → HCID 12266563, 화합물

HRID 2373138

반응식

HRID 2373138 반응식
[OH-].[Na+].[C:3]1([CH2:18]P(=O)(OCC)OCC)[CH:8]=[CH:7][C:6]([CH2:9]P(=O)(OCC)OCC)=[CH:5][CH:4]=1.[Br:27][C:28]1[CH:35]=[CH:34][C:31]([CH:32]=O)=[CH:30][CH:29]=1.O>C1C=CC=CC=1.[I-].C([N+](CCCC)(CCCC)CCCC)CCC>[Br:27][C:28]1[CH:35]=[CH:34][C:31](/[CH:32]=[CH:18]/[C:3]2[CH:4]=[CH:5][C:6](/[CH:9]=[CH:32]/[C:31]3[CH:34]=[CH:35][C:28]([Br:27])=[CH:29][CH:30]=3)=[CH:7][CH:8]=2)=[CH:30][CH:29]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 707414-BromobenzaldehydeHCID 78303Phosphonic acid, P,P'-(1,4-phenylenebis(methylene))bis-, P,P,P',P'-tetraethyl ester

생성물 1

HCID 12266563HCID 12266563, 화합물

시약·촉매·용매 2

HCID 67553Tetrabutylammonium Iodide촉매HCID 241Benzene용매

실험 절차

50% aqueous sodium hydroxide (20 ml) was added to a solution of tetraethyl p-xylylenebisphosphonate (2.40 g, 6.35 mmol) (25) and 4-bromobenzaldehyde (2.41 g, 13.02 mmol) in 10 ml of benzene. Tetra-n-butylammonium iodide (148 mmg) was added and the mixture was refluxed under nitrogen for 1 hour. The reaction mixture was allowed to cool and diluted by the addition of water (25 ml). A yellow solid was collected and washed three times with water, methanol and ether. The product was purified by recrystallization from xylenes and was isolated in 61.9% (1.73 g) yield (Product is insoluble in standard solvents).

후처리

  1. temperaturethe mixture was refluxed under nitrogen for 1 hour
  2. temperatureto cool
  3. customA yellow solid was collected
  4. washwashed three times with water, methanol and ether
  5. customThe product was purified by recrystallization from xylenes
  6. customwas isolated in 61.9% (1.73 g)
  7. customyield (Product is insoluble in standard solvents)

출처 및 근거

ORD 기록
ord-c9179945d71441d98244d7e77c38dd4d
출처 데이터셋
uspto-grants-2008_12
특허 번호
US07459106B2

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