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

HRID 1807271

반응식

HRID 1807271 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 9964566Methyl 2-ethoxy-4-nitrobenzoate수율 311%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d238a603e8ad424fabe4acc8048d82ce
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08354444B2

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