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

HRID 1296205
ノート
印刷プレビュー

反応式

HRID 1296205 の反応式
[CH3:1][O:2][C:3](=[O:20])[C:4]1[CH:9]=[C:8](C=O)[CH:7]=[CH:6][C:5]=1[O:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.[CH:21]([O:26][CH3:27])([O:24][CH3:25])OC.C(N(CC)CC)C>CO>[CH3:1][O:2][C:3](=[O:20])[C:4]1[CH:9]=[C:8]([CH:21]([O:24][CH3:25])[O:26][CH3:27])[CH:7]=[CH:6][C:5]=1[O:12][CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=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 2-benzyloxy-5-formylbenzoic acid methyl ester was dissolved in 300 ml of methanol. 60 ml of trimethyl orthoformate and 2 g of p-tosylic acid were added thereto, and the solution was heated under refluxed for 4 hours. After the solution was cooled down to room temperature, 5 ml of triethylamine was added thereto, and the solution was evaporated. The residue was dissolved in ethyl acetate, and the solution was successively washed with water and saturated sodium bicarbonate water, and dried over anhydrous magnesium sulfate, and the solvent was evaporated, to give 39.08 g of 2-(benzyloxy)-5-(dimethoxymethyl)benzoic acid methyl ester.

後処理

  1. temperaturethe solution was heated
  2. temperatureunder refluxed for 4 hours
  3. customthe solution was evaporated
  4. dissolutionThe residue was dissolved in ethyl acetate
  5. washthe solution was successively washed with water and saturated sodium bicarbonate water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-7501740c4d8044849f638aaaa096dbfb
出典データセット
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07244861B2

反応ノート

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