Acetone → 4-(3-Ethoxy-4-hydroxyphenyl)but-3-en-2-one

HRID 38667

反応式

HRID 38667 の反応式
[OH-].[Na+].[CH2:3]([O:5][C:6]1[CH:7]=[C:8]([CH:11]=[CH:12][C:13]=1[OH:14])[CH:9]=O)[CH3:4].Cl.[CH3:16][C:17]([CH3:19])=[O:18]>C(O)C.O>[CH2:3]([O:5][C:6]1[CH:7]=[C:8]([CH:9]=[CH:16][C:17](=[O:18])[CH3:19])[CH:11]=[CH:12][C:13]=1[OH:14])[CH3:4]

参加物

7

反応物 4

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 8467EthylvanillinHCID 14798Sodium Hydroxide

生成物 1

HCID 692474294-(3-Ethoxy-4-hydroxyphenyl)but-3-en-2-one収率 70.4%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

10% sodium hydroxide aqueous solution (80 ml) was added under stirring to a solution of 3-ethoxy-4-hydroxybenzaldehyde (16.6 g, 100 mmol) in acetone (50 ml), 95% ethanol (50 ml) and water (400 ml). 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 precipitated yellow solid was collected by filtration, washed with water and ethanol successively, dried, and then recrystallized from 95% ethanol to give 14.5 g of a yellow crystal, mp: 98-100° C., yield 70.4%.

後処理

  1. filtrationthe precipitated yellow solid was collected by filtration
  2. washwashed with water and ethanol successively
  3. customdried
  4. customrecrystallized from 95% ethanol

出典と根拠

ORDレコード
ord-ff7f346f666d4b05a119f33b618adecf
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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