Trifluoromethanesulfonic acid → HCID 66760033, 화합물

HRID 1850399노트

반응식

HRID 1850399 반응식
[CH3:1][O:2][C:3]1[C:8]([CH3:9])=[CH:7][C:6]([CH3:10])=[CH:5][C:4]=1[OH:11].FC(F)(F)S(O)(=O)=O>CCCCCCC>[CH3:1][O:2][C:3]1[C:4]2[O:11][C:6]([CH3:10])([CH3:7])[CH2:5][C:5]=2[C:6]([CH3:10])=[CH:7][C:8]=1[CH3:9]

참가 물질

4

반응물 2

HCID 62406Trifluoromethanesulfonic acidHCID 64514463,5-Xylenol, 2-methoxy-2회

생성물 1

HCID 66760033HCID 66760033, 화합물수율 202.3%

시약·촉매·용매 1

HCID 8900Heptane용매

반응 조건

온도
55 °C

실험 절차

Further, by using 2-methoxy-3,5-dimethylphenol (7.60 g, 41.7 mmol), synthesis was also performed according to the following method. That is, to a solution of n-heptane (76 mL) containing 2-methoxy-3,5-dimethylphenol (7.60 g, 41.7 mmol) and isobutyl aldehyde (5.71 mL, 62.6 mmol), trifluoromethanesulfonic acid (1.85 mL, 20.9 mmol) was added dropwise, and the mixture was stirred at 55° C. for 2.5 hours. After cooled to room temperature, the reaction solution was washed with water and dried using anhydrous magnesium sulfate, and then the solvent was removed under reduced pressure. The obtained residue was purified by basic silica gel chromatography (hexane-ethyl acetate 100:0) and silica gel chromatography (hexane-ethyl acetate 100:0-95:5) to give 8.70 g of the title compound (yield 100%).

후처리

  1. additionwas added dropwise
  2. temperatureAfter cooled to room temperature
  3. washthe reaction solution was washed with water
  4. customdried
  5. customthe solvent was removed under reduced pressure
  6. customThe obtained residue was purified by basic silica gel chromatography (hexane-ethyl acetate 100:0) and silica gel chromatography (hexane-ethyl acetate 100:0-95:5)

출처 및 근거

ORD 기록
ord-f701e01ed7074302b2dd7aaf0f68e0ba
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957069B2

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