関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Fluorophenyl isocyanate | HCID 70955 | — |
| 反応物 | 1,2,3,6-Tetrahydropyridin-1-amine hydrochloride | HCID 19376047 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | N-[[(4-fluorophenyl)carbamoyl]amino]-1,2,3,6-tetrahydropyridine | HCID 13534699 | 77.6% |
反応手順
N-Amino-1,2,3,6-tetrahydropyridine hydrochloride (3.42 g) was dissolved in a mixture of dioxane (30 ml) and water (20 ml). The solution was adjusted to pH 7.5 with 1N-aqueous sodium hydroxide and to the resultant mixture was added a solution of 4-fluorophenylisocyanate (0.548 g) in dioxane (5 ml). Then, the mixture was kept to pH 7.5 and stirred for 2 hours at 5° C. After evaporation of organic solvent, the crystalline product was collected by filtration and recrystallized from diisopropyl ether to give white needles of N-[[(4-fluorophenyl)carbamoyl]amino]-1,2,3,6-tetrahydropyridine (0.73 g). mp: 156°-157° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04725608 |
|---|
| 出典データセット | uspto-grants-1988_02 |
|---|
| ORD ID | ord-a3795389ab974dca90679ddbd9c6c680 |
|---|
| 出典メモ | uspto-grants-1988_02 |
|---|
