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Ethanol → Ethyl 2-hydroxy-3-nitrobenzoate

HRID 1809121
ノート
印刷プレビュー

反応式

HRID 1809121 の反応式
[OH:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[CH2:14](O)[CH3:15]>Cl>[CH2:14]([O:5][C:4](=[O:6])[C:3]1[CH:7]=[CH:8][CH:9]=[C:10]([N+:11]([O-:13])=[O:12])[C:2]=1[OH:1])[CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 702EthanolHCID 68073-Nitrosalicylic acid

生成物 1

HCID 12157235Ethyl 2-hydroxy-3-nitrobenzoate収率 86%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

10.0 g (55 mmol) of 2-hydroxy-3-nitrobenzoic acid was dissolved in 100 mL of ethanol 2 mL of concentrated hydrochloric acid was added dropwise thereto and stirred for 24 hr under heat-reflux. The mixture was cooled to room temperature and concentrated under reduced pressure, followed by dilution with ethyl acetate. The diluted solution was washed with saturated sodium bicarbonate solution and saturated sodium chloride solution, then dried over magnesium sulfate and concentrated under reduced pressure. The resulting residue was subjected to column chromatography (ethyl acetate:hexane=1:4) to obtain the title compound (10.0 g, yield: 86%).

後処理

  1. additionwas added dropwise
  2. temperatureunder heat-reflux
  3. concentrationconcentrated under reduced pressure
  4. washThe diluted solution was washed with saturated sodium bicarbonate solution and saturated sodium chloride solution
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-9a5bddc75fdd4659935320fcf0679367
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08362012B2

反応ノート

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