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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Acetone → 1,3-Dioxane-4,6-dione, 2,2-dimethyl-5-(2-propenyl)-

HRID 552035
ノート
印刷プレビュー

反応式

HRID 552035 の反応式
[CH3:1][C:2]1([CH3:11])[O:7][C:6](=[O:8])[CH:5]([CH3:9])[C:4](=[O:10])[O:3]1.[CH2:12](Br)[CH:13]=C.C(=O)([O-])[O-].[K+].[K+].CC(C)=O>C(OCC)C>[CH3:11][C:2]1([CH3:1])[O:3][C:4](=[O:10])[CH:5]([CH2:9][CH:12]=[CH2:13])[C:6](=[O:8])[O:7]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 180AcetoneHCID 7841Allyl bromideHCID 11430Potassium CarbonateHCID 772992,2,5-Trimethyl-1,3-dioxane-4,6-dione

生成物 1

HCID 112291701,3-Dioxane-4,6-dione, 2,2-dimethyl-5-(2-propenyl)-収率 94.5%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

To a 500 mL 3-necked round bottomed flask equipped with a stir bar, thermowell and a condenser connected to a nitrogen line was added 10.0 g (0.0632 mole) of 2,2,5-trimethyl-1,3-dioxane-4,6-dione, 7.7 g (0.0632 mol) of allyl bromide, 21 g (0.152 mol) of potassium carbonate and 200 mL of acetone. The mixture was refluxed with stirring overnight at which time it was allowed to cool, diluted with 200 mL of ethyl ether and filtered through a bed of Celite/activated charcoal. The filtrate was washed with water and brine and dried overnight over anhydrous sodium sulfate. The suspension was filtered and the filtrate evaporated on a rotary evaporator to yield 11 g of 2,2-dimethyl-5-allyl-1,3-dioxane-4,6-dione compound as shown in Formula (IV)) as a clear, colorless oil.

後処理

  1. customTo a 500 mL 3-necked round bottomed flask equipped with a stir bar
  2. customthermowell and a condenser connected to a nitrogen line
  3. temperatureThe mixture was refluxed
  4. temperatureto cool
  5. filtrationfiltered through a bed of Celite/activated charcoal
  6. washThe filtrate was washed with water and brine
  7. dry with materialdried overnight over anhydrous sodium sulfate
  8. filtrationThe suspension was filtered
  9. customthe filtrate evaporated on a rotary evaporator

出典と根拠

ORDレコード
ord-d0504deea8c14d0a9b0584d9eae53de1
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07951525B2

反応ノート

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