Butanedione → HCID 22320020、化合物

HRID 497578ノート

反応式

HRID 497578 の反応式
[CH:1]12[CH2:11][CH:6]3[CH2:7][CH:8]([CH2:10][CH:4]([CH2:5]3)[O:3][C:2]1=[O:12])[CH2:9]2.C[C:14](=O)[C:15](=[O:17])C.O=O>C(O)(=O)C>[C:15]([C:6]12[CH2:11][CH:1]3[CH2:9][CH:8]([CH2:10][CH:4]([O:3][C:2]3=[O:12])[CH2:5]1)[CH2:7]2)(=[O:17])[CH3:14]

参加物

5

反応物 3

HCID 650ButanedioneHCID 977OxygenHCID 5567274-Oxatricyclo[4.3.1.13,8]undecan-5-one

生成物 1

HCID 22320020HCID 22320020、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
80 °C

実験手順

In a flask were placed 3-oxatricyclo[4.3.1.14,8]undecan-2-one (16.6 g, 100 mmol), acetylacetonatocobalt [Co(acac)2] (50 mmol), 2,3-butanedione (600 mmol), and acetic acid (100 g). A condenser and an oxygen balloon were attached to the flask, and the mixture in the flask was vigorously stirred at 80° C. for 4 hours. After the completion of the reaction, the reaction mixture was concentrated, followed by addition of toluene and washing with water. The resulting organic layer was concentrated, the concentrate was subjected to silica gel column chromatography and thereby yielded the title compound 6-acetyl-3-oxatricyclo[4.3.1.14,8]undecan-2-one in a yield of 37%.

後処理

  1. customIn a flask were placed
  2. customAfter the completion of the reaction
  3. concentrationthe reaction mixture was concentrated
  4. additionfollowed by addition of toluene
  5. washwashing with water
  6. concentrationThe resulting organic layer was concentrated

出典と根拠

ORDレコード
ord-213326070c114b72a4f86b8e608c703b
出典データセット
uspto-grants-2005_09
特許番号
US06949615B2

反応ノート

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