Allyl bromide → HCID 23117635、化合物

HRID 1178322ノート

反応式

HRID 1178322 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].[OH-].[Na+].[CH2:25](Br)[CH:26]=[CH2:27].S([O-])([O-])(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.C([N+](CCCC)(CCCC)CCCC)CCC>C(Cl)Cl>[CH:15](=[N:14][C:5]([C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[C:8]([Cl:13])[CH:7]=1)([CH2:27][CH:26]=[CH2:25])[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 4

HCID 7841Allyl bromideHCID 14798Sodium HydroxideHCID 11433187Bis(tetrabutylammonium) sulphateHCID 58696280HCID 58696280、化合物

生成物 1

HCID 23117635HCID 23117635、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Ethyl(benzylidene-amino)-(3,4-dichlorophenyl)acetate (425 g) was dissolved in methylene chloride (1.8 L). 10N Aqueous sodium hydroxide (1.2 L), allyl bromide (158 mL), and tetrabutylammonium sulfate (41 g) were added to the resultant solution, followed by stirring at room temperature for one hour. The reaction mixture was subjected to partitioning. Water (1 L) was added to the aqueous layer, and then the mixture was extracted with methylene chloride. The thus-obtained organic layer was washed with saturated brine, dried over sodium sulfate anhydrate, and concentrated under reduced pressure, to thereby give the title compound (518 g). The title compound was used in the next step without further purification.

後処理

  1. customto partitioning
  2. additionWater (1 L) was added to the aqueous layer
  3. extractionthe mixture was extracted with methylene chloride
  4. washThe thus-obtained organic layer was washed with saturated brine
  5. dry with materialdried over sodium sulfate anhydrate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-1c53244836ad429c81e46983e8c7443d
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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