化工社化工社 化学情報印刷レポート · 研究参考用
Methyl acetoacetate → 4-Hydroxy-6-[2-(4-hydroxy-phenyl)-ethyl]-6-methyl-5,6-dihydro-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 | 4-(4-tert-Butyldimethylsilyloxy-phenyl)-2-butanone | HCID 18798666 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 4-Hydroxy-6-[2-(4-hydroxy-phenyl)-ethyl]-6-methyl-5,6-dihydro-pyran-2-one | HCID 54682278 | — |
反応手順
The title compound was prepared as described in General Method 6 using 16.9 g (60.9 mmol) of 4-(4-tert-butyldimethylsilyloxyphenyl)-2-butanone (prepared in Example R), 7.32 g (183 mmol) of 60% NaH dispersion in mineral oil, 21.2 g (183 mmol) of methyl acetoacetate, 114 mL (1.64M, 183 mmol) of n-butyllithium and 360 mL of THF. The reaction mixture was quenched with 0.1N HCl and the product was extracted into EtOAc. The organic layer was dried (MgSO4) and the solvents were evaporated.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05834506 |
| 出典データセット | uspto-grants-1998_11 |
| ORD ID | ord-e209b0bc14a640bf9248b15e91816ead |
| 出典メモ | uspto-grants-1998_11 |