関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2,2,2-Trifluoroethanol | HCID 6409 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2,2,2-Trifluoroethanol sodium salt | HCID 86742142 | — |
| 反応物 | 1-[(6-chloropyridin-3-yl)methyl]-N-nitroimidazolidin-2-imine | HCID 135527764 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 1-[2-(2,2,2-Trifluoroethoxy)-5-pyridylmethyl]-2-(nitroimino)imidazolidine | HCID 136342790 | 23.6% |
反応手順
Sodium hydride (0.48 g) was added to a solution of 2,2,2-trifluoroethanol (2.4 g) in toluene (30 ml) was added, and the mixture was stirred until the generation of hydrogen ceased. As a result, 2,2,2-trifluoroethanol sodium salt was prepared. To the product were added 1-(2-chloro-5-pyridylmethyl)-2-(nitroimino)imidazolidine (5.1 g) synthesized by the method of Example 3 and a catalytic amount of 4-dimethylaminopyridine. The mixture was heated at 80° C. for 10 hours with stirring. After cooling the reaction mixture, the precipitated crystals were collected by filtration, washed with water and ether and then purified by silica gel chromatography to give 1-[2-(2,2,2-trifluoroethoxy)-5-pyridylmethyl]-2-(nitroimino)imidazolidine (1.5 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05428032 |
|---|
| 出典データセット | uspto-grants-1995_06 |
|---|
| ORD ID | ord-37f501ed7b344cf2b37eaf2f0fd15b97 |
|---|
| 出典メモ | uspto-grants-1995_06 |
|---|
