Allyl bromide → HCID 23117635, 화합물

HRID 1178322노트

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HRID 1178322 반응식
[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

참가 물질

6

반응물 4

HCID 7841Allyl bromideHCID 14798Sodium HydroxideHCID 11433187Bis(tetrabutylammonium) sulphateHCID 58696280HCID 58696280, 화합물

생성물 1

HCID 23117635HCID 23117635, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1c53244836ad429c81e46983e8c7443d
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07276511B2

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