関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 18-Crown-6 | HCID 28557 | — |
| 反応物 | 2-Nitro-1-propene | HCID 78486 | — |
| 反応物 | 2,2,5,5-Tetramethylcyclopentan-1-ol | HCID 551696 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 13878919 | HCID 13878919 | — |
反応手順
2,2,5,5-Tetramethyl-1-cyclopentanol is added to a dry flask under argon at 0° C. Dry tetrahydrofuran is added with a syringe. Sodium hydride (60% dispersion in oil) is added quickly in one portion and the contents of the flask are stirred for one hour at room temperature. A 10 mM solution of 18-crown-6-ether in acetonitrile is added with a syringe and the flask cooled to 0° C. A tetrahydrofuran solution of 2-nitropropene is added with vigorous stirring over a 10 minute period. After completion of the reaction as judged by thin layer chromatography, it is quenched with saturated ammonium chloride and extracted with ethyl acetate. The organic layer is dried over MgSO4 and evaporated to yield 1-(2-nitropropoxy)-2,2,5,5-tetramethylcyclopentane.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04698231 |
|---|
| 出典データセット | uspto-grants-1987_10 |
|---|
| ORD ID | ord-f06c1869e41f41c888d338b2f2c8b765 |
|---|
| 出典メモ | uspto-grants-1987_10 |
|---|