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

HRID 2361329

反応式

HRID 2361329 の反応式
[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]

参加物

3

反応物 2

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

生成物 1

HCID 273300Methyl 2,5-dimethylbenzoate収率 82.4%

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-dca110198fd24d218f488171ec343e3b
出典データセット
uspto-grants-2014_04
特許番号
US08685969B2

関連ノート

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