化工社化工社 化学情報印刷レポート · 研究参考用
Methyl acetoacetate → 5,6-Dihydro-6-phenyl-6-(2-phenylethyl)-2H-pyran-2-one
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 | Dihydrochalcone | HCID 64802 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 5,6-Dihydro-6-phenyl-6-(2-phenylethyl)-2H-pyran-2-one | HCID 21222418 | — |
反応手順
The title compound was prepared as described in General Method 1 using 25 mmol of methyl acetoacetate, 27.5 mmol of NaH 60% dispersion in oil, 26.25 mmol of 1.6M n-butyl lithium in hexane, 25 mmol of 3-phenylpropiophenone and 70 mL of tetrahydrofuran. Upon concentrating the reaction a solid precipitated out which was triturated with ether and filtered (m.p. 130°-130.55,° C.). 1H NMR (CDCl3) δ 2.2-2.4 (m, 2 H), 2.4-2.6 (m, 1 H), 2.6-2.8 (m, 1 H), 2.9 (d, 1 H), 3.0 (d, 1 H), 3.3 (d, 1 H), 3.4 (d, 1 H), 7.0-7.5 (m, 15 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 |
| ORD ID | ord-775cf00caf8847c0a60c4dc573089d9b |
| 出典メモ | uspto-grants-1998_11 |