2,4-Dimethylbenzoic acid → Methyl 2,4-dimethylbenzoate

HRID 1625870

반응식

HRID 1625870 반응식
[CH3:1][C:2]1[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[C:12](Cl)(=O)C(Cl)=O>C(Cl)(Cl)Cl.CN(C)C=O>[CH3:1][C:2]1[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:3]=1[C:4]([O:6][CH3:12])=[O:5]

참가 물질

5

반응물 2

HCID 118972,4-Dimethylbenzoic acidHCID 65578Oxalyl chloride

생성물 1

HCID 32031Methyl 2,4-dimethylbenzoate

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매HCID 6212Chloroform용매

실험 절차

2,4-dimethylbenzoic acid (20.0 g) was suspended in chloroform (100 ml), and thereto were added oxalyl chloride (6.8 ml) and N,N-dimethylformamide (2 drops). The mixture was stirred at room temperature overnight. The solvent was evaporated under reduced pressure, and the residue was dissolved in methanol (200 ml). The mixture was stirred at room temperature for 3 hours. The solvent was evaporated under reduced pressure, and the residue was dissolved in ethyl acetate. The mixture was washed successively with a saturated aqueous sodium hydrogen carbonate solution and brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure to give methyl 2,4-dimethylbenzoate as pale yellow oil, which was used in the subsequent step without further purification.

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionthe residue was dissolved in methanol (200 ml)
  3. stirringThe mixture was stirred at room temperature for 3 hours
  4. customThe solvent was evaporated under reduced pressure
  5. dissolutionthe residue was dissolved in ethyl acetate
  6. washThe mixture was washed successively with a saturated aqueous sodium hydrogen carbonate solution and brine
  7. dry with materialdried over sodium sulfate
  8. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-b9fa98f2bcf44b5cabbfc1ecb919a6f0
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785403B2

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