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Dimethylformamide → Methyl 3-acetyl-4-methoxybenzoate

HRID 1003354
ノート
印刷プレビュー

反応式

HRID 1003354 の反応式
[C:1]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=1O)[C:7]([OH:9])=[O:8])(=[O:3])[CH3:2].CI.[C:16](=O)([O-])[O-].[K+].[K+].CN([CH:25]=[O:26])C>>[C:1]([C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=1[O:26][CH3:25])[C:7]([O:9][CH3:16])=[O:8])(=[O:3])[CH3:2]
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 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 91792453-Acetyl-4-hydroxybenzoic acid

生成物 1

HCID 10798398Methyl 3-acetyl-4-methoxybenzoate

実験手順

3-Acetyl-4-hydroxybenzoic acid (3.60 g, 20 mmol) and methyl iodide (5.68 g, 40 mmol) were dissolved in 60 ml of DMF, followed by the addition of 11.06 g (80 mmol) of potassium carbonate. The resulting mixture was stirred at room temperature for 2 hours. The DMF was distilled off under reduced pressure, followed by the addition of water. The resulting mixture was extracted with chloroform. The organic layer was dried over MgSO4, the solvent was distilled off under reduced pressure, and the residue was recrystallized from acetone-hexane, whereby 1.42 g of the title compound were obtained as brown powder (yield: 34%).

後処理

  1. distillationThe DMF was distilled off under reduced pressure
  2. additionfollowed by the addition of water
  3. extractionThe resulting mixture was extracted with chloroform
  4. dry with materialThe organic layer was dried over MgSO4
  5. distillationthe solvent was distilled off under reduced pressure
  6. customthe residue was recrystallized from acetone-hexane

出典と根拠

ORDレコード
ord-0babf8cb5bcb46ebbe683ced8c096fac
出典データセット
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06046212

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート