Potassium Carbonate → 5'-Chloro-2'-(2-methyl-2-propenyloxy)acetophenone

HRID 416025

반응식

HRID 416025 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([OH:11])=[C:6]([C:8](=[O:10])[CH3:9])[CH:7]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:19][C:20]([CH3:22])=[CH2:21]>CN(C)C=O.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:11][CH2:21][C:20]([CH3:22])=[CH2:19])=[C:6]([C:8](=[O:10])[CH3:9])[CH:7]=1

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 740613-Chloro-6-hydroxyacetophenoneHCID 3577853-Bromo-2-methyl-1-propene

생성물 1

HCID 582940385'-Chloro-2'-(2-methyl-2-propenyloxy)acetophenone수율 97.9%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
60 °C

실험 절차

A suspension of 5′-chloro-2′-hydroxyacetophenone (0.86 g, 5.0 mmol), potassium carbonate (1.4 g, 10 mmol) and 3-bromo-2-methylpropene (0.56 mL, 5.5 mmol) in anhydrous N,N-dimethylformamide (20 mL) was stirred at 60° C. for 4 hours. After cooling, the reaction mixture was diluted with water (100 mL), and the whole was extracted with ethyl acetate (100 mL). The organic layer was washed with saturated aqueous ammonium chloride solution (50 mL) and brine (50 mL) and dried over anhydrous magnesium sulfate. The solvent was removed in vacuo to give the title reference compound (1.1 g) as orange oil (Yield 96%).

후처리

  1. temperatureAfter cooling
  2. extractionthe whole was extracted with ethyl acetate (100 mL)
  3. washThe organic layer was washed with saturated aqueous ammonium chloride solution (50 mL) and brine (50 mL)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-1609479122814f759c812f9af7a87ca2
출처 데이터셋
uspto-grants-2012_01
특허 번호
US08088817B2

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