Di-i-propylphosphine → HCID 178460670、化合物

HRID 1072269ノート

反応式

HRID 1072269 の反応式
O[CH2:2][C-:3]1[CH:7]=[CH:6][C:5]([CH2:8]O)=[CH:4]1.[CH-:10]1[CH:14]=[CH:13][CH:12]=[CH:11]1.[Fe+2:15].[CH:16]([PH:19][CH:20]([CH3:22])[CH3:21])([CH3:18])[CH3:17]>C(O)(=O)C>[CH:16]([P:19]([CH2:2][C-:3]1[CH:7]=[CH:6][C:5]([CH2:8][P:19]([CH:14]([CH3:13])[CH3:10])[CH:16]([CH3:18])[CH3:17])=[CH:4]1)[CH:20]([CH3:22])[CH3:21])([CH3:18])[CH3:17].[CH-:10]1[CH:14]=[CH:13][CH:12]=[CH:11]1.[Fe+2:15]

参加物

4

反応物 2

HCID 536496Di-i-propylphosphineHCID 1296777371,3-Bis-(hydroxymethyl)ferrocene

生成物 1

HCID 178460670HCID 178460670、化合物収率 175.6%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
80 °C

実験手順

2.46 g (10 mmol) of 1,3-bis(hydroxymethyl)ferrocene and 4.72 g (40 mmol) of diisopropylphosphine were added to 40 ml of acetic acid. The resulting mixture was heated at 80° C. for 3.5 hours and extracted with benzene after cooling. The organic phase was then washed with water and then dried over Na2SO4. After evaporation an orange residue was chromatographed on an alumina column. Elution with an ether-light petroleum mixture yielded 3.92 g (88%) of the product. Selected NMR data (CDCl3, 22° C.) 1H: δ0.92 (m, 24H, CH3), 1.63 (m, 4H, CH(CH3)2), 2.49 (bs, 4H, CH2P), 3.92 (s, 5H, C5H5), 3.95 (bs, 2H, 4.5-H), 4.06 (bs, 1H, 2-H). 31P NMR (CDCl3, 22° C.): δ 10.97(s, 2P).

後処理

  1. extractionextracted with benzene
  2. temperatureafter cooling
  3. washThe organic phase was then washed with water
  4. dry with materialdried over Na2SO4
  5. customAfter evaporation an orange residue
  6. customwas chromatographed on an alumina column
  7. washElution with an ether-light petroleum mixture

出典と根拠

ORDレコード
ord-96bf738a4d2c4a24a3ffaab036618fc6
出典データセット
uspto-grants-2005_06
特許番号
US06909009B2

反応ノート

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