関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 2,4-Dichlorophenethyl alcohol | HCID 2734099 | — |
| 反応物 | Diethyl azodicarboxylate | HCID 5462977 | — |
| 反応物 | Methyl 4-chloro-3-hydroxybenzoate | HCID 11819787 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Chloro-3-[2-(2,4-dichloro-phenyl)-ethoxy]-benzoic Acid Methyl Ester | HCID 69652287 | — |
反応手順
2.0 g (10.72 mmol) of 4-Chloro-3-hydroxy-benzoic acid methyl ester was dissolved in 20 ml of anhydrous tetrahydrofuran. To this solution was added 2.25 g (11.79 mmol) of 2-(2,4-Dichlorophenyl)-ethanol, 10.71 g (equivalent to 32.2 mmol PPh3) of triphenylphosphine derivatized polystyrene and 5.6 g (32.2 mmol) of DEAD. The solution was shaken for 16 h at RT. The polymer was filtered off and washed with ethyl acetate. The solvent was removed under reduced pressure. The residue was taken-up in ethyl acetate and the solution was washed three times with water and twice with saturated aqueous sodium chloride. The organic phase was dried with magnesium sulphate, filtered and the solvent was removed under reduced pressure. The residue was chromatographed on silica gel eluting with ethyl acetate/n-heptane (1/6).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06953857B2 |
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| 出典データセット | uspto-grants-2005_10 |
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| ORD ID | ord-b316ee85efe943cba3f6ed291f32e5cb |
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| 出典メモ | uspto-grants-2005_10 |
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