関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nicotinic Acid | HCID 938 | — |
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 反応物 | Tryptamine hydrochloride | HCID 67652 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | Tryptamide | HCID 65768 | 72.5% |
反応手順
To a solution of 1.97 g (10 mmol) of tryptamine hydrochloride and 1.23 g (10 mmol) of nicotinic acid in 10 ml of dry pyridine at 0° C. were added 2.20 g (10.7 mmol) of dicyclohexylcarbodiimide. The reaction mixture was stirred at room temperature for 24 hrs, and the formed dicyclohexylurea was removed by filtration (2.34 g). The pyridine was removed in vacuo, and 10 ml of methanol were added to the residue. Insoluble dicyclohexylurea in methanol was removed by filtration (0.05 g). The methanol was removed in vacuo and 10 ml of methylene chloride was added to the residue. Insoluble compound in methylene chloride was removed by filtration (0.04 g). The methylene chloride was removed in vacuo and the residue was crystallized from isopropanol. Recrystallization from methanol/isopropanol gave 1.92 g (72.5%) of N-[2-(3-indolyl)ethyl]nicotinamide as pale brown plates, m.p. 150°-152° C. IR (KBr) 3280, 3050, 2940, 1646, 1526, 1412, 1302, 1102, 740, 697 cm-1. Anal. calc. for C16H15N3O: C, 72.42; H, 5.91; N, 15.84. Found: C, 72.51; H, 5.74; N, 15.77.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04900837 |
|---|
| 出典データセット | uspto-grants-1990_02 |
|---|
| ORD ID | ord-8a7a940126f04220a56d642959f3863d |
|---|
| 出典メモ | uspto-grants-1990_02 |
|---|