Methanol → Cyclohexylfulvene

HRID 1251529ノート

反応式

HRID 1251529 の反応式
[CH:1]1[CH2:5][CH:4]=[CH:3][CH:2]=1.[C:6]1(=O)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1.CO.N1CCC[CH2:16]1>O.C(O)(=O)C>[CH:6]1([C:2]2[C:1](=[CH2:16])[CH:5]=[CH:4][CH:3]=2)[CH2:11][CH2:10][CH2:9][CH2:8][CH2:7]1

参加物

7

反応物 4

HCID 887MethanolHCID 7612CyclopentadieneHCID 7967CyclohexanoneHCID 31268Pyrrolidine

生成物 1

HCID 22327799Cyclohexylfulvene収率 92.8%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

8.2 ml (100 mmol) of cyclopentadiene and 4.2 ml (40 mmol) of cyclohexanone were added to 40 ml of dehydrated methanol, and 5.0 ml (60 mmol) of pyrrolidine were then added dropwise at 0° C. Then, reaction was carried out at room temperature for 3 hours. Next, 3.8 ml of acetic acid were slowly added at 0° C., and 20 ml of water were further added, followed by extraction with diethyl ether. The resultant organic phase, after washed with water, was dried over magnesium sulfate, and the used solvent was then distilled off to obtain 5.95 g of a yellow liquid.

後処理

  1. additionwere then added dropwise at 0° C
  2. customThen, reaction
  3. extractionfollowed by extraction with diethyl ether
  4. washThe resultant organic phase, after washed with water
  5. dry with materialwas dried over magnesium sulfate
  6. distillationthe used solvent was then distilled off

出典と根拠

ORDレコード
ord-ac64bae7b4274fdc8052ee9019980cbe
出典データセット
uspto-grants-2002_01
特許番号
US06342568B1

反応ノート

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