化工社化工社 化学情報印刷レポート · 研究参考用
3,4-Dimethylbenzoic acid → 3,4-Dimethyl-5-nitrobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3,4-Dimethylbenzoic acid | HCID 12073 | — |
| 反応物 | Potassium nitrite | HCID 516910 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 3,4-Dimethyl-5-nitrobenzoic acid | HCID 11367572 | 48.1% |
反応手順
A solution of 3,4-dimethylbenzoic acid (40 g) in concentrated sulphuric acid (250 ml) was cooled to 0° C., treated with a solution of potassium nitrite (27 g) in sulphuric acid (100 ml) dropwise over a period of 1 h, and stirred for 2 h. The reaction mixture was quenched with ice cooled water (100 ml). The solid precipitated was filtered, dissolved in water (2 l), basified with 2N aqueous sodium hydroxide. The solution was acidified to pH 4 with 2N aqueous hydrochloric acid and filtered to get 3,4-dimethyl-5-nitrobenzoic acid (II) (25 g) as colorless solid. The filtrate was further acidified to pH 3 and filtered get 3,4-dimethyl-2-nitrobenzoic acid (I) (13 g) as colorless solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08859592B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-c0cac1017daf4671a2aa47d3bf6ad083 |
| 出典メモ | uspto-grants-2014_10 |