2,5-Dimethylbenzoic acid → Methyl 2,5-dimethylbenzoate

HRID 2361329

반응식

HRID 2361329 반응식
[CH3:1][C:2]1[CH:10]=[CH:9][C:8]([CH3:11])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].Cl.O1CCOC[CH2:14]1>>[CH3:1][C:2]1[CH:10]=[CH:9][C:8]([CH3:11])=[CH:7][C:3]=1[C:4]([O:6][CH3:14])=[O:5]

참가 물질

3

반응물 2

HCID 118922,5-Dimethylbenzoic acidHCID 204431481,4-Dioxane hydrochloride

생성물 1

HCID 273300Methyl 2,5-dimethylbenzoate수율 82.4%

실험 절차

A colorless, homogeneous solution of 2,5-dimethylbenzoic acid (6.3264 g, 42.1 mmol) and 4 N HCl/1,4-dioxane (11.58 mL, 46.3 mmol) was refluxed under nitrogen. After 2.5 hr, the reaction was cooled to room temperature and concentrated in vacuo. The residue was dissolved in EtOAc (100 mL) and washed with water (40 mL), 1N aq. NaOH (40 mL), water (40 mL) and brine (40 mL), successively. The organic solution was dried over MgSO4 and concentrated in vacuo to give the desired product (5.934 g, 34.7 mmol, 82% yield) as a colorless oil.

후처리

  1. concentrationconcentrated in vacuo
  2. dissolutionThe residue was dissolved in EtOAc (100 mL)
  3. washwashed with water (40 mL), 1N aq. NaOH (40 mL), water (40 mL) and brine (40 mL)
  4. dry with materialThe organic solution was dried over MgSO4
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-dca110198fd24d218f488171ec343e3b
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08685969B2

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