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Potassium Carbonate → Methyl 2-(2-cyanophenoxy)acetate

HRID 540346
ノート
印刷プレビュー

反応式

HRID 540346 の反応式
[OH:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]#[N:5].C(=O)([O-])[O-].[K+].[K+].Br[CH2:17][C:18]([O:20][CH3:21])=[O:19]>CC(C)=O>[C:4]([C:3]1[CH:6]=[CH:7][CH:8]=[CH:9][C:2]=1[O:1][CH2:17][C:18]([O:20][CH3:21])=[O:19])#[N:5]
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 11430Potassium CarbonateHCID 119072-HydroxybenzonitrileHCID 60984Methyl bromoacetate

生成物 1

HCID 1472933Methyl 2-(2-cyanophenoxy)acetate収率 61.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To the mixture of 2-hydroxybenzonitrile (40 g, 0.34 mol) and potassium carbonate (51.6 g, 0.374 mol) in 850 mL of acetone was added methyl bromoacetate (51.7 g, 0.34 mol) slowly at room temperature. After being stirred at room temperature overnight, the solid was filtered off. The filtrate was concentrated under reduced pressure and the residue was dissolved in ethyl acetate. The organic layer was washed with water then brine, dried over sodium sulfate, filtered and concentrated under reduced pressure to give a residue which was recrystallized in methanol to give 40 g of product as a white solid.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. filtrationthe solid was filtered off
  2. concentrationThe filtrate was concentrated under reduced pressure
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washThe organic layer was washed with water
  5. dry with materialbrine, dried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customto give a residue which
  9. customwas recrystallized in methanol

出典と根拠

ORDレコード
ord-fd675ce6c38641f58bafe201b6bda07b
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08871756B2

反応ノート

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