関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Methyl 2-methyl-3-nitrobenzoate | HCID 601165 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-Amino-2-methylbenzoic acid methyl ester | HCID 3801025 | 82.1% |
反応手順
40 g of methyl 2-methyl-3-nitrobenzoate was dissolved in 120 ml of methanol, and 157 g of concentrated hydrochloric acid was added thereto. Then, 36.8 g of iron powder was gradually added while maintaining the mixture at a temperature of not higher than 60° C. The mixture was stirred at room temperature for 4 hours and then poured into 1 liter of ice water. The solution was neutralized with sodium carbonate and extracted with chloroform (after filtering off insolubles). The extract was washed with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate. Then, the solvent was distilled off to obtain 27.8 g of the desired product as an oily substance.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04885022 |
|---|
| 出典データセット | uspto-grants-1989_12 |
|---|
| ORD ID | ord-2cd6a3df76fe4a0d85dd76b53090eeaa |
|---|
| 出典メモ | uspto-grants-1989_12 |
|---|