Dimethyl Sulfate → 4-(4-Methoxy-3-ethoxyphenyl)-3-buten-2-one

HRID 38666

反応式

HRID 38666 の反応式
[C:1](=O)([O-])[O-].[Na+].[Na+].S(OC)(OC)(=O)=O.[OH:14][C:15]1[CH:20]=[CH:19][C:18]([CH:21]=[CH:22][C:23](=[O:25])[CH3:24])=[CH:17][C:16]=1[O:26][CH2:27][CH3:28]>CC(C)=O>[CH3:1][O:14][C:15]1[CH:20]=[CH:19][C:18]([CH:21]=[CH:22][C:23](=[O:25])[CH3:24])=[CH:17][C:16]=1[O:26][CH2:27][CH3:28]

参加物

5

反応物 3

HCID 6497Dimethyl SulfateHCID 10340Sodium CarbonateHCID 692474294-(3-Ethoxy-4-hydroxyphenyl)but-3-en-2-one

生成物 1

HCID 539602744-(4-Methoxy-3-ethoxyphenyl)-3-buten-2-one収率 65.3%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Anhydrous sodium carbonate (3.98 g) and dimethyl sulfate (3.78 g, 30 mmol) were added to a solution of 4-(4-hydroxy-3-ethoxyphenyl)-3-buten-2-one (6.2 g, 30 mmol) in acetone (40 ml). The reaction mixture was stirred under refluxing for 8 hr. The precipitated yellow solid was filtered, washed with acetone, and then recrystallized from anhydrous ethanol to give 4.3 g of a yellow crystal, mp 95-96° C., yield 65.3%.

後処理

  1. temperatureunder refluxing for 8 hr
  2. filtrationThe precipitated yellow solid was filtered
  3. washwashed with acetone
  4. customrecrystallized from anhydrous ethanol

出典と根拠

ORDレコード
ord-78ec42e1d23b4d7b91bc52b5997e61ff
出典データセット
uspto-grants-2013_09
特許番号
US08524744B2

関連ノート

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