化工社化工社 化学情報印刷レポート · 研究参考用
p-Toluenesulfonic acid → 1-{6-[1-(2-Isopropyl-6-methyl-phenylimino)-ethyl]-pyridin-2-yl}-ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | 2,6-Diacetylpyridine | HCID 70790 | — |
| 反応物 | 6-Isopropyl-o-toluidine | HCID 78920 | — |
| 溶媒 | 1-Propanol | HCID 1031 | — |
| 生成物 | 1-{6-[1-(2-Isopropyl-6-methyl-phenylimino)-ethyl]-pyridin-2-yl}-ethanone | HCID 86674240 | — |
反応手順
1-(6-Acetyl-pyridin-2-yl)-ethanone 2 (35.54 g, 0.22 mol), 25.0 g (0.168 mol) of 2-Isopropyl-6-methyl-phenylamine 14, 350 ml of n-propanol, and a few crystals of p-toluenesulfonic acid were stirred at room temperature for 36 h in a 500 ml flask under a flow of the nitrogen. The resultant yellow precipitate was filtered and washed by 20 ml of methanol. It was then dried at 1-mm vacuum overnight. The yield of 1-{6-[1-(2-Isopropyl-6-methyl-phenylimino)-ethyl]-pyridin-2-yl}-ethanone 15 was 13.35 g (27%) as a yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09175104B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-fe2da5511576423d8abec7f0d5365048 |
| 出典メモ | uspto-grants-2015_11 |