Acetone → 4-(3-Methoxy-4-ethoxyphenyl)-3-buten-2-one

HRID 38668

반응식

HRID 38668 반응식
[OH-].[Na+].[CH3:3][O:4][C:5]1[CH:6]=[C:7]([CH:10]=[CH:11][C:12]=1[O:13][CH2:14][CH3:15])[CH:8]=O.Cl.[CH3:17][C:18]([CH3:20])=[O:19]>C(O)C.O>[CH3:3][O:4][C:5]1[CH:6]=[C:7]([CH:8]=[CH:17][C:18](=[O:19])[CH3:20])[CH:10]=[CH:11][C:12]=1[O:13][CH2:14][CH3:15]

참가 물질

7

반응물 4

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 671164-Ethoxy-3-methoxybenzaldehyde

생성물 1

HCID 692481204-(3-Methoxy-4-ethoxyphenyl)-3-buten-2-one수율 66.5%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

10% sodium hydroxide aqueous (40 ml) was added under stirring to a solution of 3-methoxy-4-ethoxybenzaldehyde (9.09 g, 50 mmol) in acetone (25 ml), 95% ethanol (25 ml) and water (200 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 solid was collected by filtrating and washed with water and ethanol successively, dried, and then recrystallized from 95% ethanol to give 7.38 g of a pale yellow solid, mp: 95-97° C., yield: 66.5%.

후처리

  1. customThe precipitated solid was collected
  2. filtrationby filtrating
  3. washwashed with water and ethanol successively
  4. customdried
  5. customrecrystallized from 95% ethanol

출처 및 근거

ORD 기록
ord-494e067128284a1eb05853ce0472705c
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524744B2

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