化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Carbonate → Methyl 3-amino-2-methyl-6-thiocyanatobenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Sodium Bromide | HCID 253881 | — |
| 反応物 | Sodium thiocyanate | HCID 516871 | — |
| 反応物 | 3-Amino-2-methylbenzoic acid methyl ester | HCID 3801025 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Methyl 3-amino-2-methyl-6-thiocyanatobenzoate | HCID 14801188 | 91.2% |
反応手順
While maintaining a solution comprising 27.7 g of methyl 3-amino-2-methylbenzoate, 41.5 g of sodium thiocyanate and 250 ml of methanol at a temperature of not higher than 0° C., 100 ml of sodium bromide-saturated methanol with 28.1 g of bromine was slowly dropwise added thereto. The mixture was stirred at room temperature for 3 hours and then poured into 1 liter of ice water. The solution was neutralized with sodium carbonate and then extracted with chloroform. 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 34.0 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-787fce87cce8402592768e9530675cb5 |
| 出典メモ | uspto-grants-1989_12 |