Trifluoromethanesulfonic acid → HCID 66760033、化合物

HRID 1850399ノート

反応式

HRID 1850399 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 66760033HCID 66760033、化合物収率 202.3%

試薬・触媒・溶媒 1

HCID 8900Heptane溶媒

反応条件

温度
55 °C

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-f701e01ed7074302b2dd7aaf0f68e0ba
出典データセット
uspto-grants-2015_02
特許番号
US08957069B2

反応ノート

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