関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Ammonium Bicarbonate | HCID 14013 | — |
| 反応物 | 2,3,5-Trimethyl-1-oxidopyridin-1-ium | HCID 10486907 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-Nitro-2,3,5-trimethylpyridine, 1-oxide | HCID 11217611 | 81.5% |
反応手順
To 98% sulfuric acid (4.93 kg, 49.3 mol), 2,3,5-trimethylpyridine1-oxide (1.38 kg, 10.1 mol) was added. After 97% nitric acid (1.44 kg) was added dropwise thereto over 50 minutes, the mixture was heated at 85° C. for 4 hours. The reaction mixture was poured to a mixture of ammonium hydrogen carbonate (10.6 kg) and water (9.0 L). The mixture was extracted with ethyl acetate (3.0 L×3). The obtained organic layer was concentrated and dried under vacuum overnight to obtain a desired product (1.50 kg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07425634B2 |
|---|
| 出典データセット | uspto-grants-2008_09 |
|---|
| ORD ID | ord-96c5b1cc39524b49a713b86ca5077f65 |
|---|
| 出典メモ | uspto-grants-2008_09 |
|---|
