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Pinacolone → 8-Methoxy-2,2-dimethyloctan-3,5-dione

HRID 2200785
ノート
印刷プレビュー

反応式

HRID 2200785 の反応式
[H-].[Na+].C[O:4][CH2:5][CH2:6][CH2:7][C:8]([O:10][CH3:11])=O.[C:12]([C:16]([CH3:18])=[O:17])([CH3:15])([CH3:14])[CH3:13]>COCCOC>[CH3:11][O:10][CH2:8][CH2:7][CH2:6][C:5](=[O:4])[CH2:18][C:16](=[O:17])[C:12]([CH3:15])([CH3:14])[CH3:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6416PinacoloneHCID 24758Sodium hydrideHCID 542317Methyl 4-methoxybutanoate

生成物 1

HCID 129919568-Methoxy-2,2-dimethyloctan-3,5-dione収率 14%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

1.8 mol of sodium hydride was added to the solvent ethylene glycol dimethyl ether, and 1 mol of methyl 4-methoxybutanoate was added thereto and stirred at room temperature for 10 minutes. Then, 1.2 mol of t-butylmethylketone was added to the solution which was then stirred at 92° C. for 19 hours. Then, the solution was cooled to room temperature and quenched in 36% hydrochloric acid, after which water and dimethylether were added to and mixed with the solution, and water was removed therefrom. The resulting organic material was washed with 1 wt % sodium hydroxide and then with saturated saline and concentrated, and the residue was fractionated, thereby obtaining the intermediate 8-methoxy-2,2-dimethyloctan-3,5-dione at a yield of 14%.

後処理

  1. additionwas added
  2. stirringwas then stirred at 92° C. for 19 hours
  3. temperatureThen, the solution was cooled to room temperature
  4. customquenched in 36% hydrochloric acid
  5. additionafter which water and dimethylether were added to and
  6. additionmixed with the solution, and water
  7. customwas removed
  8. washThe resulting organic material was washed with 1 wt % sodium hydroxide
  9. concentrationwith saturated saline and concentrated

出典と根拠

ORDレコード
ord-a42c55caeb4c4777a5edffb39a37c8f5
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09359382B2

反応ノート

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