Bis(eta-cyclopentadienyl) iron → HCID 178520645、化合物

HRID 259288

反応式

HRID 259288 の反応式
[CH-:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1.[CH-:6]1[CH:10]=[CH:9][CH:8]=[CH:7]1.[Fe+2:11].[Cl:12][CH2:13][CH2:14][C:15](Cl)=[O:16].[Cl-].[Al+3].[Cl-].[Cl-]>ClCCl>[Cl:12][CH2:13][CH2:14][C:15]([C-:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1)=[O:16].[CH-:6]1[CH:10]=[CH:9][CH:8]=[CH:7]1.[Fe+2:11]

参加物

5

反応物 3

HCID 7611Bis(eta-cyclopentadienyl) ironHCID 693643-Chloropropionyl chlorideHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 178520645HCID 178520645、化合物収率 89.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of ferrocene (2.63 kg, 14.2 mole) and 3-chloropropionyl chloride (1.8 kg, 15.6 moles) in dry dichloromethane (23.5 l) was cooled to -3° and treated over 1 hour with aluminium chloride (2.08 kg, 15.6 mole). The reaction mixture was left to stir for 2 hours. To this was then added ice water (30 kg) and the two layers separated. The aqueous layer was washed with dichloromethane and the combined organic liquors were washed with water (30 l), 2% aqueous sodium bicarbonate solution (20 l) and water again (60 l). The organic liquors were then dried and concentrated affording black/brown semi-solid chloropropionyl ferrocene (3.5 kg).

後処理

  1. waitThe reaction mixture was left
  2. customadded ice water (30 kg) and the two layers separated
  3. washThe aqueous layer was washed with dichloromethane
  4. washthe combined organic liquors were washed with water (30 l), 2% aqueous sodium bicarbonate solution (20 l) and water again (60 l)
  5. customThe organic liquors were then dried
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-ad264747c90646f39039de9bd0e79dc8
出典データセット
uspto-grants-1977_07
特許番号
US04036983

関連ノート

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