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Methane → 2-[(Butylamino)(butylimino)methylthio]-3-quinoxalinecarboxylic acid ethyl ester, hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methane | HCID 297 | — |
| 反応物 | N,N'-Dibutylthiourea | HCID 2723622 | — |
| 反応物 | Ethyl 3-Chloroquinoxaline-2-carboxylate | HCID 12283436 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 2-[(Butylamino)(butylimino)methylthio]-3-quinoxalinecarboxylic acid ethyl ester, hydrochloride | HCID 131712839 | 47.5% |
反応手順
2-Chloro-3-quinoxalinecarboxylic acid ethyl ester (7.10 g., 0.03 mole) was dissolved in 125 ml. of acetone treated with Norit and filtered. The filtrate was added to 5.650 g. (0.03 mole) of 1,3-di-n-butylthiourea in 100 ml. of acetone. The solution was stirred at reflux under a nitrogen atmosphere for 6 hours, allowed to cool to room temperature, and stirred an additional 17 hours. The red solution was treated with Norit, filtered, and concentrated to a volume of 100 ml. The yellow solid that crystallized out was collected by filtration, washed and dried to give the 6.05 g. (47.5% yield) of product, m.p. 138°-139° C. (dec.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04349674 |
| 出典データセット | uspto-grants-1982_09 |
| ORD ID | ord-f825206e528846759b677540039b12f1 |
| 出典メモ | uspto-grants-1982_09 |