化工社化工社 化学情報印刷レポート · 研究参考用
2-Methylbenzenesulfonic acid → 2-Phthalimidoethyl acetoacetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Methylbenzenesulfonic acid | HCID 6925 | — |
| 反応物 | N-(2-Hydroxyethyl)phthalimide | HCID 77499 | — |
| 反応物 | 2,2,6-Trimethyl-4H-1,3-dioxin-4-one | HCID 79368 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-Phthalimidoethyl acetoacetate | HCID 11403106 | 76.4% |
反応手順
A solution of 10.0 g (52.3 mmol) of N-(2-hydroxyethyl)phthalimide, 8.84 ml (67.7 mmol) of 2,2,6-trimethyl-1,3-dioxen-4-one, and 10 mg of p toluenesulfonic acid in 50 ml of toluene is heated at reflux under N2 for 4 hr. The solvent is removed under vacuum and the dark-colored residue is flash chromatographed on silica gel (1:1 hexane-EtOAc). The resulting product is recrystallized from EtOAc to give 11.0 g of 2-phthalimidoethyl acetoacetate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05258519 |
| 出典データセット | uspto-grants-1993_11 |
| ORD ID | ord-7987d50d9c2949d8bba937edd21fb7c1 |
| 出典メモ | uspto-grants-1993_11 |