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

HRID 982215ノート

反応式

HRID 982215 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

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.

後処理

  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))

出典と根拠

ORDレコード
ord-df6a8e50177342358c61bf1bab0e83df
出典データセット
uspto-grants-1991_02
特許番号
US04994479

反応ノート

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