4-Dimethylaminoacetophenone → (2E)-3-(dimethylamino)-1-[4-(dimethylamino)phenyl]prop-2-en-1-one

HRID 514390

반응식

HRID 514390 반응식
[CH3:1][N:2]([CH3:12])[C:3]1[CH:8]=[CH:7][C:6]([C:9](=[O:11])[CH3:10])=[CH:5][CH:4]=1>CN(C(OC)OC)C.C1(C)C=CC=CC=1.CC(O)=O>[CH3:1][N:2]([CH3:12])/[CH:3]=[CH:10]/[C:9]([C:6]1[CH:7]=[CH:8][C:3]([N:2]([CH3:1])[CH3:12])=[CH:4][CH:5]=1)=[O:11]

참가 물질

5

반응물 1

HCID 750374-Dimethylaminoacetophenone

생성물 1

HCID 71285027(2E)-3-(dimethylamino)-1-[4-(dimethylamino)phenyl]prop-2-en-1-one수율 35.8%

시약·촉매·용매 3

HCID 176Acetic Acid촉매HCID 1140Toluene용매HCID 78373Dimethylformamide dimethyl acetal용매

실험 절차

A solution of 1-[4-(dimethylamino)phenyl]ethanone (500 mg, 3.1 mmol) in DMF-DMA (10 mL), toluene (10 mL), and AcOH (2 drops), was heated under reflux conditions for 48 h. The solution was concentrated and purified by flash column chromatography (hexanes:EtOAc=8:2˜1:1) to give the title compound (121 mg, 18%) as a yellow solid.

후처리

  1. concentrationThe solution was concentrated
  2. custompurified by flash column chromatography (hexanes:EtOAc=8:2˜1:1)

출처 및 근거

ORD 기록
ord-902f43f21db94618b0be5351002cdefa
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09107916B2

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