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Aluminum(III) Chloride → HCID 178519740、化合物

HRID 1657509
ノート
印刷プレビュー

反応式

HRID 1657509 の反応式
[C-:1]1([C:6]([CH2:8][CH2:9][CH2:10][CH2:11][C:12]([Cl:14])=O)=[O:7])[CH:5]=[CH:4][CH:3]=[CH:2]1.[CH-:15]1[CH:19]=[CH:18][CH:17]=[CH:16]1.[Fe+2:20].[Cl-].[Al+3].[Cl-].[Cl-]>C(Cl)Cl>[Cl:14][C:12]1[CH2:11][CH2:10][CH2:9][C:8]=1[C:6]([C-:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1)=[O:7].[CH-:15]1[CH:19]=[CH:18][CH:17]=[CH:16]1.[Fe+2:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6451240Aluminum(III) ChlorideHCID 178521142HCID 178521142、化合物

生成物 1

HCID 178519740HCID 178519740、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

This brown oil (ferrocenoyl valeroyl chloride) assumed to be 0.01 mole from the above preparation in methylene chloride (100 ml) was stirred at 0°-5° and aluminium chloride (1.3g; 0.01 mole) was added. Ice was then added and the organic layer was separated. The aqueous layer was extracted with chloroform. The combined organic fractions were washed with water, dried (magnesium sulphate) and evaporated to yield a red oil which was purified by dry-column chromatography on silica, which had been deactivated to Grade III by the addition of water, using 1:10 ethylacetate: petroleum ether as eluent, to yield pure 1-chloro-2-ferrocenoylcyclopent-1-ene, 150 mg; mp 102°.

後処理

  1. additionIce was then added
  2. customthe organic layer was separated
  3. extractionThe aqueous layer was extracted with chloroform
  4. washThe combined organic fractions were washed with water
  5. dry with materialdried (magnesium sulphate)
  6. customevaporated
  7. customto yield a red oil which
  8. customwas purified by dry-column chromatography on silica, which
  9. additionhad been deactivated to Grade III by the addition of water

出典と根拠

ORDレコード
ord-018b1124b69b499592cac7fe47d77c70
出典データセット
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03960911

反応ノート

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