関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2-(3-Methoxyphenyl)-1-phenylethan-1-one | HCID 2759614 | — |
| 反応物 | Lithium bis(trimethylsilyl)amide | HCID 57426343 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Ethyl 4-(m-methoxyphenyl)-3-phenyl-3-hydroxybutyrate | HCID 22602685 | 86% |
反応手順
Lithium hexamethyidisilazane (88.5 mL, 88.5 mmol) was added to THF (150 mL) at −78° C. After 15 minutes, ethyl acetate (7.79 g, 88.5 mmol) was added over 10 minutes and stirred at −78° C. for 30 minutes. The m-methoxybenzyl phenyl ketone in (10.0 g, 44.25 mmol) THF (100 mL) was added over 15 minutes and kept at that temperature for 3 hours. The reaction mixture was quenched at that temperature with saturated ammonium chloride (15 mL). The reaction mixture was diluted with ether (200 mL) and the organic layer was washed with brine, (100 mL), dried and concentrated to afford the desired product (12 g, 86% yield). NMR was consistent with the desired structure.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06720315B2 |
|---|
| 出典データセット | uspto-grants-2004_04 |
|---|
| ORD ID | ord-0d7cb346805c40b583610cf6d62715e4 |
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| 出典メモ | uspto-grants-2004_04 |
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