Acetic Acid → 2,6,6-Trimethylfulvene

HRID 271026

反応式

HRID 271026 の反応式
[CH3:1][C:2]1[CH2:6][CH:5]=[CH:4][CH:3]=1.[CH3:7][C:8]([CH3:10])=O.N1CCCC1.C(O)(=O)C>CCOCC.O.CO>[CH3:1][C:2]1[CH:6]=[CH:5][C:4](=[C:8]([CH3:10])[CH3:7])[CH:3]=1

参加物

8

反応物 4

HCID 176Acetic AcidHCID 180AcetoneHCID 31268PyrrolidineHCID 667751-Methyl-1,3-cyclopentadiene

生成物 1

HCID 143632822,6,6-Trimethylfulvene収率 92.5%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

To 130 ml of dehydrated methanol, 22.6 g (283 mmol) of methylcyclopentadiene and 8.50 ml (116 mmol) of acetone were added, then 14.5 ml (174 mmol) of pyrrolidine was dropwise added at 0° C., and the mixture was reacted at room temperature for one night. Then, 10 ml (180 mmol) of acetic acid was added at 0° C. The mixture was diluted with ether and water and then subjected to extraction. Then, the organic phase was separated, washed with water and dried over anhydrous magnesium sulfate to obtain 12.9 g of a brown liquid. The analyzed values are given below.

後処理

  1. customthe mixture was reacted at room temperature for one night
  2. extractionsubjected to extraction
  3. customThen, the organic phase was separated
  4. washwashed with water
  5. dry with materialdried over anhydrous magnesium sulfate

出典と根拠

ORDレコード
ord-02e1cd6f9c1b4900b49a714d7d59086e
出典データセット
uspto-grants-2008_11
特許番号
US07449533B2

関連ノート

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