関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | N,N'-Dimethylethylenediamine | HCID 8070 | — |
| 反応物 | (4-Bromo-2-methylphenyl)-[2-(4-methylpiperidin-1-yl)ethyl]amine | HCID 69054033 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | (4-Iodo-2-methylphenyl)-[2-(4-methylpiperidin-1-yl)ethyl]amine | HCID 69059102 | — |
反応手順
73 mg (0.386 mmol) of CuI, 1.16 g (7.71 mmol) of NaI, and N,N′-dimethylethane-1,2-diamine were added under argon to a solution of 1.20 g (3.86 mmol) of (4-bromo-2-methylphenyl)-[2-(4-methylpiperidin-1-yl)ethyl]amine in 3.9 mL of 1,4-dioxane and the mixture was stirred for 20 hours at 110° C. The reaction mixture was cooled to RT and diluted with EtOAc. The organic phase was washed with 10% aqueous ammonia, dried over magnesium sulfate, and evaporated down in vacuo. Yield: 1.22 g (88% of theoretical); C15H23IN2 (M=358.261); calc.: molpeak (M+H)+: 359; found: molpeak (M+H)+: 359; HPLC-MS: 6.24 minutes (method A).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07592358B2 |
|---|
| 出典データセット | uspto-grants-2009_09 |
|---|
| ORD ID | ord-80f30f2375254e768b98961b4ae5f607 |
|---|
| 出典メモ | uspto-grants-2009_09 |
|---|
