関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | HCID 57586512 | HCID 57586512 | — |
| 反応物 | HCID 178502985 | HCID 178502985 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 57586498 | HCID 57586498 | 71.3% |
反応手順
To a 0° C. solution of 4-[2-(2-Ethoxycarbonyl-ethyl)-3-(6-oxo-hexyl)-phenoxy]-butyric acid ethyl ester (7.0 g, 17.24 mmol) and potassium carbonate (7.14 g, 51.72 mmol) in MeOH (200 mL), the Ohira's reagent (ref. cited in Synlett, 1996, 521) (6.3 g, 32.8 mmol) in MeOH (50 mL) was added slowly. The cooling bath was removed upon the end of addition and the reaction mixture stirred at room temperature for 5 hr. The reaction was then extracted with EtOAc and brine. The combined organic layers were dried over sodium sulfate then evaporated under vacuo. The crude material was purified by column chromatography using 50% EtOAc-Hexane as eluant to give the title compound (4.6 g, 71%) as a light yellow oil. HR-ES(+): calculated for C22H30O5 (M+Na)1+ 397.1985, found 397.1985.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08093385B2 |
|---|
| 出典データセット | uspto-grants-2012_01 |
|---|
| ORD ID | ord-c283fb61c69a4aafb6146e4644833d3c |
|---|
| 出典メモ | uspto-grants-2012_01 |
|---|