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Methanol → 1-(3-Chlorophenyl)ethanone

HRID 727179
ノート
印刷プレビュー

反応式

HRID 727179 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 13015Benzonitrile, m-chloro-HCID 178418573HCID 178418573、化合物

生成物 1

HCID 149331-(3-Chlorophenyl)ethanone

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1518c00294774bacbe3ba301d4199895
出典データセット
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05712281

反応ノート

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