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Methanol → 1-(3-Chlorophenyl)ethanone

HRID 727179
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HRID 727179 반응식
[CH3:1][Mg]Br.[Cl:4][C:5]1[CH:6]=[C:7]([CH:10]=[CH:11][CH:12]=1)C#N.[CH3:13][OH:14]>O1CCCC1>[Cl:4][C:5]1[CH:12]=[C:11]([C:13]([CH3:1])=[O:14])[CH:10]=[CH:7][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 887MethanolHCID 13015Benzonitrile, m-chloro-HCID 178418573HCID 178418573, 화합물

생성물 1

HCID 149331-(3-Chlorophenyl)ethanone

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Under a nitrogen atmosphere, 36.7 mL (0.11 mole) of methylmagnesium bromide (3.0M in diethyl ether) is stirred, and a solution of 13.8 grams (0.10 mole) of 3-chlorobenzonitrile in 50 mL of dry tetrahydrofuran is added slowly dropwise. Upon completion of addition, the reaction mixture is warmed to reflux where it is stirred for about 18 hours. After this time the reaction mixture is cooled to ambient temperature, and about 40 mL of methanol is added dropwise. Upon completion of addition, the reaction mixture is stirred for two hours and then filtered. The filtrate is then stirred for about 18 hours with 35 grams of silica gel and 100 mL of water. The mixture is filtered, and the filtrate is diluted with ethyl acetate. The mixture is then washed with water, and the organic layer is dried with magnesium sulfate. The mixture is filtered, and the filtrate is concentrated under reduced pressure, yielding methyl 3-chlorophenyl ketone.

후처리

  1. additionUpon completion of addition
  2. temperaturethe reaction mixture is warmed
  3. temperatureto reflux where it
  4. additionUpon completion of addition
  5. stirringthe reaction mixture is stirred for two hours
  6. filtrationfiltered
  7. stirringThe filtrate is then stirred for about 18 hours with 35 grams of silica gel and 100 mL of water
  8. filtrationThe mixture is filtered
  9. additionthe filtrate is diluted with ethyl acetate
  10. washThe mixture is then washed with water
  11. dry with materialthe organic layer is dried with magnesium sulfate
  12. filtrationThe mixture is filtered
  13. concentrationthe filtrate is concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-1518c00294774bacbe3ba301d4199895
출처 데이터셋
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05712281

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