化工社化工社 化学情報印刷レポート · 研究参考用
alpha-Cyclohexylcyclohexanemethanamine → N,N-Dicyclohexylmethyl-N',N'-dibenzyl-2-butene-1,4-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | alpha-Cyclohexylcyclohexanemethanamine | HCID 10774245 | — |
| 反応物 | 1-Acetoxy-4-dibenzylamino-2-butene | HCID 53789779 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N,N-Dicyclohexylmethyl-N',N'-dibenzyl-2-butene-1,4-diamine | HCID 57036974 | — |
反応手順
A solution of 1-acetoxy-4-dibenzylamino-2-butene (10.1 g, 33 mmol) and dicyclohexylmethylamine (6.8 g, 32 mmol) in 50 ml of THF is treated with tetrakis(triphenylphosphine)palladium(0) (1.0 g, 0.9 mmol) and stirred at room temperature overnight. The reaction mixture is concentrated in vacuo to a solid which is redissolved in 100 ml of THF and treated with 25 ml of 20% aqueous sodium hydroxide. The mixture is stirred for one hour, concentrated and extracted with diethyl ether. The ether extracts are dried and concentrated to give a solid which is then purified by crystallization from isopropanol. The title compound is obtained in a yield of 9.7 g (65%) as a white solid melting at 61°-62° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05391808 |
| 出典データセット | uspto-grants-1995_02 |
| ORD ID | ord-0c0a7f9cdbb94fbaab85f436ddbb5d29 |
| 出典メモ | uspto-grants-1995_02 |