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

HRID 1816597
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반응식

HRID 1816597 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d536531e4ee24836b302493058a25f53
출처 데이터셋
uspto-grants-2005_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06884821B1

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