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

HRID 38670
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인쇄 미리보기

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HRID 38670 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

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

생성물 1

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

시약·촉매·용매 1

HCID 702
Ethanol
용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-58ff3b5366694c5a9b29089b2dce39a1
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08524744B2

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