p-Toluenesulfonic acid monohydrate → Methyl 2-ethoxy-4-nitrobenzoate

HRID 1807271

反応式

HRID 1807271 の反応式
[CH2:1]([O:3][C:4]1[CH:12]=[C:11]([N+:13]([O-:15])=[O:14])[CH:10]=[CH:9][C:5]=1[C:6]([OH:8])=[O:7])[CH3:2].O.[C:17]1(C)C=CC(S(O)(=O)=O)=CC=1>CO>[CH2:1]([O:3][C:4]1[CH:12]=[C:11]([N+:13]([O-:15])=[O:14])[CH:10]=[CH:9][C:5]=1[C:6]([O:8][CH3:17])=[O:7])[CH3:2]

参加物

4

反応物 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 27363472-Ethoxy-4-nitrobenzoic acid

生成物 1

HCID 9964566Methyl 2-ethoxy-4-nitrobenzoate収率 311%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 2-ethoxy-4-nitrobenzoic acid (2.035 g, 9.45 mmol, Aldrich) in methanol (40 ml) was treated with p-toluenesulfonic acid monohydrate (583.3 mg, 3.07 mmol) and heated at reflux under argon for 17 hrs. The solvent was removed and the residue was dissolved in ethyl acetate, washed with saturated Na2CO3, water and saturated NaCl and dried over Na2SO4, filtered and concentrated to give methyl 2-ethoxy-4-nitrobenzoate (2.15 g, 101%) as a yellow solid.

後処理

  1. temperatureheated
  2. temperatureat reflux under argon for 17 hrs
  3. customThe solvent was removed
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. washwashed with saturated Na2CO3, water and saturated NaCl
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-d238a603e8ad424fabe4acc8048d82ce
出典データセット
uspto-grants-2013_01
特許番号
US08354444B2

関連ノート

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