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Dimethyl Sulfate → HCID 54346298、化合物

HRID 2228843
ノート
印刷プレビュー

反応式

HRID 2228843 の反応式
[CH3:1][C:2](=[CH2:10])[CH2:3][C:4](=[N:8][OH:9])[C:5](=[O:7])[CH3:6].[C:11](=O)([O-])[O-].[K+].[K+].S(OC)(OC)(=O)=O>CC(C)=O>[CH3:11][O:9][N:8]=[C:4]([CH2:3][C:2]([CH3:1])=[CH2:10])[C:5](=[O:7])[CH3:6]
参加物反応条件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 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 73447335HCID 73447335、化合物

生成物 1

HCID 54346298HCID 54346298、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒2 回

反応条件

温度
23 °C

実験手順

141 g of 5-methylhex-5-ene-2,3-dione 3-oxime from Example 1 were dissolved in 750 ml of acetone and admixed with 165.6 g of potassium carbonate. 145 g of dimethyl sulfate in 100 ml of acetone were then added dropwise, and the mixture was stirred at 23° C. for 4 hours. The solvent was then removed under reduced pressure, the residue was taken up in methyl tert-butyl ether/water and the aqueous phase was extracted repeatedly with methyl tert-butyl ether. The combined organic phases were washed with 15% strength ammonia solution and water and dried over sodium sulfate, and the solvent was removed under reduced pressure. This gave 141 g of the title compound as a yellow oil.

後処理

  1. customThe solvent was then removed under reduced pressure
  2. extractionthe aqueous phase was extracted repeatedly with methyl tert-butyl ether
  3. washThe combined organic phases were washed with 15% strength ammonia solution and water
  4. dry with materialdried over sodium sulfate
  5. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-8c2576f1c1024a5eaea3aca0da6d1d41
出典データセット
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06417388B1

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート