化工社化工社 化学情報印刷レポート · 研究参考用
Thionyl Chloride → 3,5-Diamino-2-methylbenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 3,4-Diaminobenzoic acid | HCID 69263 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3,5-Diamino-2-methylbenzoic acid | HCID 135524 | 81% |
反応手順
To dry methanol (20 ml) was carefully added thionyl chloride (1 ml) dropwise with stirring. The 3,4-diaminobenzoic acid (1 g) was added in portions at R.T. with stirring then the mixture heated at reflux for 3 h. Saturated sodium bicarbonate was added until the mixture was basic, then the mixture extracted into chloroform containing 25% methanol. The extract was dried and evaporated in vacuo to give the product (0.88 g, 81%) as a brown crystalline solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07745490B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-79f45971a6444b508008851ae0cf9325 |
| 出典メモ | uspto-grants-2010_06 |