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

HRID 1244278

反応式

HRID 1244278 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-17e97e05510a410c844a6f801b6189d6
出典データセット
uspto-grants-2006_10
特許番号
US07122544B2

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