Water → HCID 12266563、化合物

HRID 2373138

反応式

HRID 2373138 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 12266563HCID 12266563、化合物

試薬・触媒・溶媒 2

HCID 67553Tetrabutylammonium Iodide触媒HCID 241Benzene溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-c9179945d71441d98244d7e77c38dd4d
出典データセット
uspto-grants-2008_12
特許番号
US07459106B2

関連ノート

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