Water → 2,3,5-Trimethylphenyl acetate

HRID 2424305노트

반응식

HRID 2424305 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 136963592,3,5-Trimethylphenyl acetate수율 101.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-81fa83ef1f4648469370c96f58dccdd6
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07964531B2

반응 노트

불러오는 중…