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Triethylamine → Methyl 2-(benzyloxy)-5-(dimethoxymethyl)benzoate

HRID 1816597
ノート
印刷プレビュー

反応式

HRID 1816597 の反応式
[CH2:1]([O:8][C:9]1[CH:18]=[CH:17][C:16](C=O)=[CH:15][C:10]=1[C:11]([O:13][CH3:14])=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:21]([O:26][CH3:27])([O:24][CH3:25])OC.C(N(CC)CC)C>CO>[CH2:1]([O:8][C:9]1[CH:18]=[CH:17][C:16]([CH:21]([O:24][CH3:25])[O:26][CH3:27])=[CH:15][C:10]=1[C:11]([O:13][CH3:14])=[O:12])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 9005Trimethyl orthoformateHCID 22494045Methyl 2-(benzyloxy)-5-formylbenzoate

生成物 1

HCID 22494305Methyl 2-(benzyloxy)-5-(dimethoxymethyl)benzoate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

39.1 g of methyl 2-benzyloxy-5-formyl-benzoate was dissolved in 300 ml methanol. 60 ml trimethyl orthoformate and 2 g of p-toluenesulffonic acid were added thereto, followed by heating under reflux for 4 hours. After cooling to room temperature, 5 ml triethylamine was added thereto, and the mixture was evaporated. The residue was dissolved in ethyl acetate, successively washed with water and saturated aqueous sodium bicarbonate solution, dried over anhydrous magnesium sulfate and the solvent was evaporated, to give 39.08 g of methyl 2-(benzyloxy)-5-(dimethoxymethyl)benzoate.

後処理

  1. temperatureby heating
  2. temperatureunder reflux for 4 hours
  3. customthe mixture was evaporated
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. washsuccessively washed with water and saturated aqueous sodium bicarbonate solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-d536531e4ee24836b302493058a25f53
出典データセット
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06884821B1

反応ノート

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