化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 2-(4-Chlorobutyramido)-4-methyloxazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-Chlorobutyryl chloride | HCID 78370 | — |
| 反応物 | 4-Methyloxazol-2-amine | HCID 535824 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | 2-(4-Chlorobutyramido)-4-methyloxazole | HCID 21323645 | 23.92% |
反応手順
2-Amino-4-methyloxazole (5.0 g., 0.0509 mol) was dissolved in dry benzene (100 mls.) and triethylamine (5.70 g., 0.0563 mol) was added. The mixture was stirred vigorously at room temperature and 4-chlorobutyrylchloride (7.88 g., 0.0558 mol) in dry benzene (50 mls.) was added rapidly. After the addition the mixture was heated under reflux for 2 hours. The mixture was then cooled and filtered. The filtrate was placed in a separating funnel and washed successively with water (1 × 100 mls.), 10% Na2CO3 (2 × 100 mls.) and water (3 × 100 mls.). The organic layer was dried over magnesium sulphate and evaporated under vacuum. The product was recrystallised from ethyl acetate/hexane. Wt. = 2.47 g.m.p. 98° C. (Yield = 23.92%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04150143 |
| 出典データセット | uspto-grants-1979_04 |
| ORD ID | ord-d462603abd2e427f959d6ea4f0629ee8 |
| 出典メモ | uspto-grants-1979_04 |