Water → Ethyl 5-(p-heptyloxybenzyloxy)-1-methoxy-2-indaneacetate

HRID 982215노트

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HRID 982215 반응식
[OH:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[CH:7]([O:11][CH3:12])[CH:6]([CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:5]2.[CH2:19]([O:26][C:27]1[CH:34]=[CH:33][C:30]([CH2:31]Cl)=[CH:29][CH:28]=1)[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O.C(OCC)(=O)C>[CH2:19]([O:26][C:27]1[CH:34]=[CH:33][C:30]([CH2:31][O:1][C:2]2[CH:3]=[C:4]3[C:8](=[CH:9][CH:10]=2)[CH:7]([O:11][CH3:12])[CH:6]([CH2:13][C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:5]3)=[CH:29][CH:28]=1)[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]

참가 물질

7

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 14674285p-Heptyloxybenzyl chlorideHCID 54284451Ethyl 5-hydroxy-1-methoxyindane-2-acetate

생성물 1

HCID 53634688Ethyl 5-(p-heptyloxybenzyloxy)-1-methoxy-2-indaneacetate수율 63.8%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

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온도
60 °C

실험 절차

In 2 ml of dimethylformamide were dissolved 190 mg of ethyl 5-hydroxy-1-methoxyindane-2-acetate and 220 mg of p-heptyloxybenzyl chloride. To the solution was added 180 mg of potassium carbonate. The mixture was stirred at 60° C. overnight. After allowing to cool, water and ethyl acetate were added to the mixture. By thoroughly shaking the mixture, the organic layer was separated. After washing with water, drying and concentrating the organic layer, the residue obtained was purified by flash chromatography (eluant: toluene/ethyl acetate (25/1)) to obtain 220 mg of ethyl 5-(p-heptyloxybenzyloxy)-1-methoxy-2-indaneacetate as a colorless oily product.

후처리

  1. temperatureto cool
  2. stirringBy thoroughly shaking the mixture
  3. customthe organic layer was separated
  4. washAfter washing with water
  5. customdrying
  6. concentrationconcentrating the organic layer
  7. customthe residue obtained
  8. customwas purified by flash chromatography (eluant: toluene/ethyl acetate (25/1))

출처 및 근거

ORD 기록
ord-df6a8e50177342358c61bf1bab0e83df
출처 데이터셋
uspto-grants-1991_02
특허 번호
US04994479

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