Di-i-propylphosphine → HCID 178460670, 화합물

HRID 1072269노트

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HRID 1072269 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 178460670HCID 178460670, 화합물수율 175.6%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
80 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-96bf738a4d2c4a24a3ffaab036618fc6
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06909009B2

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