Bis(eta-cyclopentadienyl) iron → HCID 178520645, 화합물

HRID 259288

반응식

HRID 259288 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 178520645HCID 178520645, 화합물수율 89.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-ad264747c90646f39039de9bd0e79dc8
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04036983

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