関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methyl acetoacetate | HCID 7757 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Pentafluorobenzaldehyde | HCID 69558 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 5,6-Dihydro-4-hydroxy-6-(pentafluorophenyl)-2H-pyran-2-one | HCID 54721680 | — |
反応手順
The title compound was prepared as described in General Method 1 using 2.5 mL of methyl acetoacetate, 1.0 g of NaH 60% dispersion in oil, 12.5 mL of 2.0M n-butyl lithium in hexane, 3.4 mL of pentafluorobenzaldehyde and 75 mL of tetrahydrofuran. After addition of the aldehyde, the reaction was stirred for 10 minutes at 0° C. then allowed to warm to room temperature overnight. The crude product was triturated from diethyl ether to afford a solid (m.p. 176°-178° C.). 1H NMR (CDCl3) δ 2.89 (dd, 1 H), 3.15 (dd, 1 H), 3.70 (dd, 2 H), 6.02 (dd, 1 H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05840751 |
|---|
| 出典データセット | uspto-grants-1998_11 |
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| ORD ID | ord-3e032f68de824e6ea046a4d2fb67e0a0 |
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| 出典メモ | uspto-grants-1998_11 |
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