P-Chloroacetophenone → (E)-1-(4-chlorophenyl)-3-(dimethylamino)prop-2-en-1-one

반응식

[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:10])[CH3:9])=[CH:4][CH:3]=1.C(O[CH:15](OC(C)C)[N:16]([CH3:18])[CH3:17])(C)C>>[CH3:15][N:16]([CH3:18])/[CH:17]=[CH:9]/[C:8]([C:5]1[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=1)=[O:10]

참가 물질

반응물 2

HCID 7467P-Chloroacetophenone

HCID 87682N,N,N-trimethyl-1,1-bis(1-methylethoxy)amine

생성물 1

HCID 5375260(E)-1-(4-chlorophenyl)-3-(dimethylamino)prop-2-en-1-one수율 99%

실험 절차

A solution of 1-(4-chlorophenyl)ethane-1-one (35.0 g, 226 mmol) and N,N Dimethylformamide diisopropylacetal (35 mL) was heated to reflux for 16 hours. The reaction mixture was cooled to room temperature and treated with hexanes (50 mL). The resulting solid was collected via filtration and washed with hexanes to provide the title compound as a yellow solid (47.12 g, 99% yield): HPLC Retention Time; 6.45 min (Method B). M+1; 209.

후처리

temperatureto reflux for 16 hours
filtrationThe resulting solid was collected via filtration
washwashed with hexanes

출처 및 근거

ORD 기록: ord-17e97e05510a410c844a6f801b6189d6
출처 데이터셋: uspto-grants-2006_10
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07122544B2

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