化工社化工社 化学情報印刷レポート · 研究参考用
Sulfuric Acid → Methyl isonicotinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Isonicotinic Acid | HCID 5922 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl isonicotinate | HCID 227085 | 71.8% |
反応手順
A suspension of 100 g of isonicotinic acid (0.812 mol) in 250 ml of methanol was stirred and cooled to 10°. To this mixture was added dropwise 125 ml of sulfuric acid during 15 min. keeping the temperature below 20°. The reaction mixture was allowed to come to room temperature and then heated under reflux for 4.5 hr. After standing overnight it was poured onto 1 kg of ice and made alkaline with 235 g of sodium carbonate. The solid was filtered off, washed with water and with ether, and discarded. The filtrate was extracted with 3×300 ml of ether. The combined organic extracts were washed with water and with brine, dried over sodium sulfate, and concentrated in vacuo to leave 80 g (65%) of crude product as a pale oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04560692 |
| 出典データセット | uspto-grants-1985_12 |
| ORD ID | ord-65b3708e0c1e499c9746b472280033f0 |
| 出典メモ | uspto-grants-1985_12 |