化工社化工社 化学情報印刷レポート · 研究参考用
Triethylamine → 3-Diazofuran-2,4-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | p-Toluenesulfonyl azide | HCID 13661 | — |
| 反応物 | Tetronic acid | HCID 521261 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Diazofuran-2,4-dione | HCID 15439113 | — |
反応手順
To tetronic acid (5.00 g, 49.9 mmol) in CH2Cl2 (250 mL) at 0° C. were added Et3N (8.3 mL, 59.6 mmol) and tosyl azide (7.37 g, 37.4 mmol). After a period of 2 h at r.t., the reaction mixture was partitioned between NH4OAc (25%) and CH2Cl2. The organic phase was dried over Na2SO4, filtered and evaporated under reduced pressure. The resulting mixture was purified by flash chromatography (20% to 35% EtOAc in Hexane) to provide 1.4 of the title compound as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06169188A |
| 出典データセット | uspto-grants-2001_01 |
| ORD ID | ord-1875ca71409049f99e8e967d3b45acaa |
| 出典メモ | uspto-grants-2001_01 |