化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → Butyl-(6-chloro-2-methyl-5-ethyl-pyrimidin-4-yl)-ethylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Butylethylamine | HCID 25914 | — |
| 反応物 | 4,6-Dichloro-5-ethyl-2-methylpyrimidine | HCID 21912425 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Butyl-(6-chloro-2-methyl-5-ethyl-pyrimidin-4-yl)-ethylamine | HCID 21912129 | 88.3% |
反応手順
A mixture of 2-methyl-5-ethyl-4,6-dichloro-pyrimidine (1.009 g, 5.28 mmol) in 5 ml of acetonitrile was treated with triethylamine (0.571 g, 5.65 mmol) and N-butyl-ethyl-amine (0.540 g, 5.31 mmol) and heated at reflux overnight. The mixture was diluted with water and dilute hydrogen chloride, and extracted with ethyl acetate. The organic layer was neutralized with saturated potassium carbonate and washed with brine, dried and concentrated to give 1.193 g of yellow oil which was purified through silica gel column chromatography to give 1.157 g (86%) of title compound as a yellow oil. 1H NMR (CDCl3) δ 0.90 (t, 3H), 1.13 (t, 3H), 1.18 (t, 3H), 1.1–1.33 (m, 2H), 1.4–1.6 (m, 2h), 2.41 (s, 3H), 2.62 (q, 2H), 3.25–3.48 (m, 4H) ppm.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07125880B1 |
| 出典データセット | uspto-grants-2006_10 |
| ORD ID | ord-77b900efa8784290b30af2029f3866e0 |
| 出典メモ | uspto-grants-2006_10 |