化工社化工社 化学情報印刷レポート · 研究参考用
Crotononitrile → 3-Methyl-2-morpholino-2-(alpha,alpha,alpha-trifluoro-m-tolyl)glutaronitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Crotononitrile | HCID 637921 | — |
| 反応物 | 2-Morpholino-2-[3-(trifluoromethyl)phenyl]acetonitrile | HCID 3694192 | — |
| 反応物 | Potassium hydroxide ethanol | HCID 21946426 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 3-Methyl-2-morpholino-2-(alpha,alpha,alpha-trifluoro-m-tolyl)glutaronitrile | HCID 12449517 | — |
反応手順
To a solution of α-(α,α,α-trifluoro-m-tolyl)-4-morpholineacetonitrile in 100 ml. of tetrahydrofuran is added 1.0 ml. of 30% KOH-ethanol solution. To the mixture is added 2.56 g. of crotononitrile and the mixture is stirred at room temperature for 18 hrs. The mixture is concentrated to dryness under vacuum and the residue is dissolved in chloroform. The solution is passed through a column of hydrous magnesium silicate. The eluent is concentrated to an oil (17.3 g) which is crystallized from hexane and recrystallized from CHCL3 -hexane to give 3-methyl-2-morpholino-2-(α,α,α-trifluoro-m-tolyl)glutaronitrile as crystals, m.p. 115°-118° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04112095 |
| 出典データセット | uspto-grants-1978_09 |
| ORD ID | ord-6baa0556377e44a7821e68c108ea8bbc |
| 出典メモ | uspto-grants-1978_09 |