Water → 2,3,5-Trimethylphenyl acetate

HRID 2424305

反応式

HRID 2424305 の反応式
[CH3:1][C:2]1[C:7]([CH3:8])=[CH:6][C:5]([CH3:9])=[CH:4][C:3]=1[OH:10].N1C=CC=CC=1.[C:17](OC(=O)C)(=[O:19])[CH3:18].O>ClCCl>[C:17]([O:10][C:3]1[CH:4]=[C:5]([CH3:9])[CH:6]=[C:7]([CH3:8])[C:2]=1[CH3:1])(=[O:19])[CH3:18]

参加物

6

反応物 4

HCID 962WaterHCID 1049PyridineHCID 7918Acetic AnhydrideHCID 127692,3,5-Trimethylphenol

生成物 1

HCID 136963592,3,5-Trimethylphenyl acetate収率 101.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In dichloromethane (150 mL) was dissolved 15.09 g (0.1108 mol) of 2,3,5-trimethylphenol, and 17.82 mL (0.2204 mol) of pyridine, then 20.78 mL (0.2202 mol) of acetic anhydride were added to the solution, and the mixture was stirred at room temperature overnight. The reaction mixture was poured into water, and extracted with dichloromethane. The organic layer was successively washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was removed, and the residue was purified by silica gel column chromatography (Wako gel C-100, hexane:ethyl acetate, gradient) to obtain 20.08 g (0.1127 mol, Yield: quantitative) of 2,3,5-trimethylphenyl acetate.

後処理

  1. extractionextracted with dichloromethane
  2. washThe organic layer was successively washed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was removed
  5. customthe residue was purified by silica gel column chromatography (Wako gel C-100, hexane:ethyl acetate, gradient)

出典と根拠

ORDレコード
ord-81fa83ef1f4648469370c96f58dccdd6
出典データセット
uspto-grants-2011_06
特許番号
US07964531B2

関連ノート

読み込み中…