Allyl bromide → HCID 23117635、化合物

HRID 1178323ノート

反応式

HRID 1178323 の反応式
[CH2:1]([O:3][C:4](=[O:22])[CH:5]([N:14]=[CH:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[C:8]([Cl:13])[CH:7]=1)[CH3:2].[CH2:23](Br)[CH:24]=[CH2:25].C(=O)([O-])[O-].[K+].[K+]>C(OCC)(=O)C.[Br-].C([N+](CCCC)(CCCC)CCCC)CCC>[CH:15](=[N:14][C:5]([C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[C:8]([Cl:13])[CH:7]=1)([CH2:25][CH:24]=[CH2:23])[C:4]([O:3][CH2:1][CH3:2])=[O:22])[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1

参加物

6

反応物 3

HCID 7841Allyl bromideHCID 11430Potassium CarbonateHCID 58696280HCID 58696280、化合物

生成物 1

HCID 23117635HCID 23117635、化合物収率 94.2%

試薬・触媒・溶媒 2

HCID 74236Tetrabutylammonium Bromide触媒HCID 8857Ethyl Acetate溶媒

実験手順

Ethyl(benzylidene-amino)-(3,4-dichlorophenyl)-acetate (1.41 mol) was dissolved in ethyl acetate (2.3 L). Allyl bromide (341 g), potassium carbonate (390 g), and tetrabutylammonium bromide (45 g) were added to the resultant mixture, followed by refluxing for 2.5 hours. The reaction mixture was left to cool to room temperature. The mixture was sequentially washed with water and saturated brine, dried over sodium sulfate anhydrate, and concentrated under reduced pressure, to thereby give the title compound (500 g, 94%).

後処理

  1. temperatureby refluxing for 2.5 hours
  2. waitThe reaction mixture was left
  3. washThe mixture was sequentially washed with water and saturated brine
  4. dry with materialdried over sodium sulfate anhydrate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-0e63fdad07464e2ba3a1878b7b301eee
出典データセット
uspto-grants-2007_10
特許番号
US07276511B2

反応ノート

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