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

HRID 33450

反応式

HRID 33450 の反応式
[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]

参加物

3

反応物 2

HCID 7467P-ChloroacetophenoneHCID 87682N,N,N-trimethyl-1,1-bis(1-methylethoxy)amine

生成物 1

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

実験手順

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.

後処理

  1. temperatureto reflux for 16 hours
  2. filtrationThe resulting solid was collected via filtration
  3. washwashed with hexanes

出典と根拠

ORDレコード
ord-7b143d0fd7a04fcfb5f097754da81e17
出典データセット
uspto-grants-2008_09
特許番号
US07429599B2

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