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Acetone → 4-(3,4-Dimethoxyphenyl)but-3-en-2-one

HRID 38670
ノート
印刷プレビュー

反応式

HRID 38670 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[CH:6]=O.O.[OH-].[Na+].Cl.[CH3:17][C:18]([CH3:20])=[O:19]>C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:6]=[CH:17][C:18](=[O:19])[CH3:20])[CH:8]=[CH:9][C:10]=1[O:11][CH3:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 962WaterHCID 8419VeratraldehydeHCID 14798Sodium Hydroxide

生成物 1

HCID 847484-(3,4-Dimethoxyphenyl)but-3-en-2-one収率 17.75%

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

実験手順

To a solution of 3, 4-dimethoxybenzaldehyde (8.31 g, 50 mmol) in acetone (25 ml) and 95% ethanol (25 ml) was added water (200 ml) under stirring. During this time white precipitated solid was formed, and 10% sodium hydroxide aqueous solution (40 ml) was added dropwise under stirring below 10° C. Then the reaction mixture was stirred for 24 hr at room temperature, after the reaction completed, the reaction mixture was neutralized with 6N hydrochloric acid to adjust pH=7.0, the prepicitated yellow solid was collected by filtration and washed with ethanol, dried , then recrystallized from 95% ethanol to give 4.16 g of a pale yellow crystal, mp: 78-80° C., yield: 17.75%.

後処理

  1. customDuring this time white precipitated solid
  2. customwas formed
  3. stirringunder stirring below 10° C
  4. stirringThen the reaction mixture was stirred for 24 hr at room temperature
  5. filtrationthe prepicitated yellow solid was collected by filtration
  6. washwashed with ethanol
  7. customdried
  8. customrecrystallized from 95% ethanol

出典と根拠

ORDレコード
ord-58ff3b5366694c5a9b29089b2dce39a1
出典データセット
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08524744B2

反応ノート

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