4-Nitrophenol → Methyl (4-nitrophenoxy)acetate

HRID 83778ノート

反応式

HRID 83778 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][CH:5]=1)([O-:3])=[O:2].C([O-])([O-])=O.[K+].[K+].Cl[CH2:18][C:19]([O:21][CH3:22])=[O:20]>CC(C)=O>[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([O:10][CH2:18][C:19]([O:21][CH3:22])=[O:20])=[CH:6][CH:5]=1)([O-:3])=[O:2]

参加物

5

反応物 3

HCID 9804-NitrophenolHCID 7295Methyl chloroacetateHCID 11430Potassium Carbonate

生成物 1

HCID 700522Methyl (4-nitrophenoxy)acetate収率 72.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a mixture of 4-nitrophenol (100 g, 719 mmol) and anhydrous K2CO3 (400 gm, 2.894 mol) in anhydrous acetone (950 ml) was added methyl chloroacetate (114 g, 1.050 moles) and refluxed for 12 hours. Acetone was distilled off and water (1500 ml) was added. Crude 7 was filtered, dried and recrystallised from a mixture of ethyl acetate:hexane (1:5) to give pure 7 (110 g, 72.5%) as a white fluffy powder with an m.p between 97-98.4° C.

後処理

  1. temperaturerefluxed for 12 hours
  2. distillationAcetone was distilled off
  3. additionwater (1500 ml) was added
  4. filtrationCrude 7 was filtered
  5. customdried
  6. customrecrystallised from a mixture of ethyl acetate:hexane (1:5)

出典と根拠

ORDレコード
ord-babbe404bc1e4121af8d645fddc011eb
出典データセット
uspto-grants-2014_09
特許番号
US08846845B2

反応ノート

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