関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Monobenzone | HCID 7638 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | Diisopropyl diazene-1,2-dicarboxylate | HCID 75555 | — |
| 反応物 | Methyl 2-chloro-3-[4-(2-hydroxyethyl)phenyl]propanoate | HCID 86600802 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | Methyl 3-(4-(2-[4-(benzyloxy)phenoxy]ethyl)phenyl)-2-chloropropanoate | HCID 86600803 | 67.1% |
反応手順
Triphenylphosphine (2.4 g, 9 mmol) was added to a solution of methyl 2-chloro-3-[4-(2-hydroxyethyl)phenyl]propanoate (2.1 g, 8.5 mmol) and 4-(benzyloxy)phenol (1.7 g, 8 mmol) in 20 ml toluene under nitrogen atmosphere. The solution was warmed to 55° C. and diisopropyl azodicarboxylate (1.8 g, 9 mmol) was added. The reaction mixture was stirred at 55° C. overnight. The mixture was allowed to cool and the solvent was evaporated under reduced pressure. The crude product was purified by flash chromatography using a 80:20 mixture of heptane and EtOAc as eluent to yield 2.28 g of the desired product (yield 61%) as colourless crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07429675B2 |
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| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-b1dbfc4476ed401d93f87254f4a51af6 |
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| 出典メモ | uspto-grants-2008_09 |
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