化工社化工社 化学情報印刷レポート · 研究参考用
Water → N-[2-(6-methyl-2-pyridyl)ethyl]phthalimide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Phthalimide | HCID 6809 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 6-Methylpyridine-2-ethanol | HCID 70283 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-[2-(6-methyl-2-pyridyl)ethyl]phthalimide | HCID 14478208 | 67% |
反応手順
45.6 g (262 mmol) of diethyl azadicarboxylate (DEAD) was added dropwise to a solution of 30.0 g (219 mmol) of 2-(6-methyl-2-pyridyl)ethanol, 38.6 g (262 mmol) of phthalimide and 68.6 g (262 mmol) of triphenylphosphine in 300 ml of tetrahydrofuran at a temperature of 15° to 25° C. The mixture was stirred overnight. Water was added to the mixture. After extraction with ethyl acetate, the organic layer was washed with water. After extraction with 2N hydrochloric acid, a 3N sodium hydroxide solution was added to the aqueous layer at 0° C. to make it alkaline. White crystals thus formed were collected by filtration to give 39.04 g (yield: 67%) of the intended compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05162347 |
| 出典データセット | uspto-grants-1992_11 |
| ORD ID | ord-b498fbd33c6a4946b1ca2e88ad04be3b |
| 出典メモ | uspto-grants-1992_11 |