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Water → Methyl 3-amino-2-methyl-6-methylthiobenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Sodium sulfide nonahydrate | HCID 73972 | — |
| 反応物 | Methyl 3-amino-2-methyl-6-thiocyanatobenzoate | HCID 14801188 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Methyl 3-amino-2-methyl-6-methylthiobenzoate | HCID 54391819 | 104.1% |
反応手順
To a solution comprising 39.5 g of sodium sulfide nonahydrate and 110 ml of water, a solution comprising 32.9 g of methyl 3-amino-2-methyl-6-thiocyanobenzoate and 300 ml of ethanol, was dropwise added. The mixture was stirred at room temperature for 1.5 hours, and then 24 g of methyl iodide was dropwise added thereto under cooling with ice. The mixture was stirred at room temperature for 2 hours and then, concentrated under reduced pressure. A saturated sodium chloride aqueous solution was added thereto, and the mixture was extracted with chloroform. The chloroform layer was dried over anhydrous sodium sulfate, and then the solvent was distilled off to obtain 30.1 g of the desired product. Oily substance.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | USRE034408 |
| 出典データセット | uspto-grants-1993_10 |
| ORD ID | ord-51109b9ee09446f59db9516630768ff3 |
| 出典メモ | uspto-grants-1993_10 |