Diethyl Ether → 3-(4-Biphenylyl)-4-(4-chlorophenyl)-2-butanone

HRID 1452412노트

반응식

HRID 1452412 반응식
[C:1]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:6]=[CH:5][C:4]([CH2:7][C:8](=[O:10])[CH3:9])=[CH:3][CH:2]=1.[Cl:17][C:18]1[CH:25]=[CH:24][C:21]([CH2:22]Cl)=[CH:20][CH:19]=1.[OH-].[Na+].C(OCC)C>O>[C:1]1([C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH:2]=[CH:3][C:4]([CH:7]([CH2:22][C:21]2[CH:24]=[CH:25][C:18]([Cl:17])=[CH:19][CH:20]=2)[C:8](=[O:10])[CH3:9])=[CH:5][CH:6]=1

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 77231-Chloro-4-(chloromethyl)benzeneHCID 14798Sodium HydroxideHCID 2193711-Biphenyl-4-yl-propan-2-one

생성물 1

HCID 190737923-(4-Biphenylyl)-4-(4-chlorophenyl)-2-butanone수율 53.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

9.93 g of 1-(4-biphenylyl)-2-propanone, 8.4 g of 4-chlorobenzyl chloride and 2.1 g of sodium hydroxide were mixed and heated for 5 hours with stirring on an oil bath of 80° to 90° C. The reaction solution was left to cool to room temperature. Then, ethyl ether and water were added thereto. The organic layer was collected by separation and then dried over anhydrous magnesium sulfate. The drying agent was separated by filtration, and then the solvent was distilled off under reduced pressure. The residue was recrystallized from hexane to obtain 8.42 g (yield: 53%) of the above-identified compound as colorless needles having a melting point of from 107° to 108.5° C.

후처리

  1. temperatureheated for 5 hours
  2. waitThe reaction solution was left
  3. customThe organic layer was collected by separation
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe drying agent was separated by filtration
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was recrystallized from hexane

출처 및 근거

ORD 기록
ord-01331d5fe3db4ed3a935a1af395d7de1
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05606101

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