Dichloroacetyl chloride → 8,8-Dichlorobicyclo[4.2.0]oct-2-en-7-one

HRID 648666ノート

反応式

HRID 648666 の反応式
[CH:1]1[CH2:6][CH2:5][CH:4]=[CH:3][CH:2]=1.[Cl:7][CH:8]([Cl:12])[C:9](Cl)=[O:10].C(N(CC)CC)C>C(OCC)C>[Cl:7][C:8]1([Cl:12])[CH:1]2[CH:2]([CH2:3][CH2:4][CH:5]=[CH:6]2)[C:9]1=[O:10]

参加物

5

反応物 3

HCID 6593Dichloroacetyl chlorideHCID 8471TriethylamineHCID 116051,3-Cyclohexadiene

生成物 1

HCID 125073478,8-Dichlorobicyclo[4.2.0]oct-2-en-7-one収率 70.5%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A mixture of 34.0 g of cyclohexadiene and 35.0 g of dichloroacetyl chloride in 300 ml of diethyl ether under nitrogen was refluxed while adding 31.5 g of triethylamine dropwise over a period of 3 hours. The mixture was then stirred at room temperature for 20 hours and filtered. The filtrate was washed with brine, 1N hydrochloric acid, saturated sodium bicarbonate and then dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure and the residue distilled to give 32 g of 8,8-dichlorobicyclo[4.2.0]oct-2-en-7-one.

後処理

  1. temperaturewas refluxed
  2. filtrationfiltered
  3. washThe filtrate was washed with brine, 1N hydrochloric acid, saturated sodium bicarbonate
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was removed under reduced pressure
  6. distillationthe residue distilled

出典と根拠

ORDレコード
ord-277163a41e704a9aa850952c3fe014ca
出典データセット
uspto-grants-1988_04
特許番号
US04735966

反応ノート

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