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Iodoethane → Tetraethyl (1-phenoxypropylidene)-bisphosphonate

HRID 569616
ノート
印刷プレビュー

反応式

HRID 569616 の反応式
[O:1]([CH:8]([P:17](=[O:24])([O:21][CH2:22][CH3:23])[O:18][CH2:19][CH3:20])[P:9](=[O:16])([O:13][CH2:14][CH3:15])[O:10][CH2:11][CH3:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+].[CH2:27](I)[CH3:28]>CN(C)C=O.C(OCC)(=O)C>[O:1]([C:8]([P:17](=[O:24])([O:21][CH2:22][CH3:23])[O:18][CH2:19][CH3:20])([P:9](=[O:16])([O:13][CH2:14][CH3:15])[O:10][CH2:11][CH3:12])[CH2:27][CH3:28])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6340IodoethaneHCID 24758Sodium hydrideHCID 54483224Tetraethyl (phenoxymethylene)-bisphosphonate

生成物 1

HCID 53742288Tetraethyl (1-phenoxypropylidene)-bisphosphonate

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Tetraethyl (phenoxymethylene)-bisphosphonate (1.14 g) was added to a suspension of 55% sodium hydride (0.15 g) in dimethylformamide (10 ml). After 45 minutes at room temperature, ethyl iodide (0.49 ml) was added, and the mixture was left overnight at room temperature, diluted with ethyl acetate and washed with 40% aqueous calcium chloride. The organic phase was dried and evaporated to leave an oil which was purified by chromatography on silica gel. The title compound was isolated as a colourless oil.

後処理

  1. waitthe mixture was left overnight at room temperature
  2. washwashed with 40% aqueous calcium chloride
  3. customThe organic phase was dried
  4. customevaporated
  5. customto leave an oil which
  6. customwas purified by chromatography on silica gel

出典と根拠

ORDレコード
ord-d3e6e6ed0a0a4afe9c17dd9befff510f
出典データセット
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04732998

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート