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(2-Methoxymethoxyphenyl)(2-hydroxy-3-methoxyphenyl)methane → (2-Hydroxyphenyl)-(2-hydroxy-3-methoxyphenyl)methane

HRID 1111284
ノート
印刷プレビュー

反応式

HRID 1111284 の反応式
COC[O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([O:18][CH3:19])[C:13]=1[OH:20]>CO.C1(C)C=CC(S(O)(=O)=O)=CC=1>[OH:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([O:18][CH3:19])[C:13]=1[OH:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 22151955(2-Methoxymethoxyphenyl)(2-hydroxy-3-methoxyphenyl)methane

生成物 1

HCID 22151938(2-Hydroxyphenyl)-(2-hydroxy-3-methoxyphenyl)methane

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6101p-Toluenesulfonic acid溶媒

実験手順

(2-Methoxymethoxyphenyl)(2-hydroxy-3-methoxyphenyl)methane (3.95 g, 14 mmol) was dissolved in 150 ml of methanol containing 0.026 g of p-toluene sulfonic acid and the mixture was heated at reflux overnight. The volatiles were then removed by evaporation under reduced pressure and the solid that remained was taken up in ether. The ethereal solution was extracted with saturated aqueous sodium bicarbonate, dried over magnesium sulfate, and concentrated by evaporation under reduced pressure. The white solid residue was dried to obtain 3.66 g (99 percent of theory) of the title compound. The proton nmr spectrum was consistent with the assigned structure.

後処理

  1. temperaturethe mixture was heated
  2. temperatureat reflux overnight
  3. customThe volatiles were then removed by evaporation under reduced pressure
  4. extractionThe ethereal solution was extracted with saturated aqueous sodium bicarbonate
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated by evaporation under reduced pressure
  7. customThe white solid residue was dried

出典と根拠

ORDレコード
ord-7cc9218b24b64759b0de983cd1e053d4
出典データセット
uspto-grants-1990_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04979978

反応ノート

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