3-Chloro-2-methyl-1-propene → HCID 334095, 화합물

HRID 1610762노트

반응식

HRID 1610762 반응식
[Br:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[C:4]([CH3:9])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:16](Cl)[C:17](=[CH2:19])[CH3:18]>CN(C)C=O.C(OCC)(=O)C>[Br:1][C:2]1[CH:3]=[C:4]([CH3:9])[CH:5]=[CH:6][C:7]=1[O:8][CH2:18][C:17]([CH3:19])=[CH2:16]

참가 물질

6

반응물 3

HCID 112413-Chloro-2-methyl-1-propeneHCID 11430Potassium CarbonateHCID 231092-Bromo-4-methylphenol

생성물 1

HCID 334095HCID 334095, 화합물수율 99%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
100 °C

실험 절차

To a solution of 2-bromo-p-cresol (10 ml, 82.7 mmol) in N,N-dimethylformamide (200 ml) were added potassium carbonate (17.2 g, 124 mmol) and methallyl chloride (9.8 ml, 99.2 mmol), and the mixture was stirred at 100° C. overnight. The mixture was diluted with ethyl acetate, and washed with water and saturated brine. The mixture was dried over anhydrous magnesium sulfate, filtered, and concentrated. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=5:1) to give 2-bromo-4-methyl-1-[(2-methyl-2-propenyl)oxy]benzene (19.67 g, 99%) as a colorless transparent oil.

후처리

  1. washwashed with water and saturated brine
  2. dry with materialThe mixture was dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=5:1)

출처 및 근거

ORD 기록
ord-345d97f6946146b3bbbc6dee738d4065
출처 데이터셋
uspto-grants-2006_01
특허 번호
US06982348B2

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