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Triethylamine → N-[6-(n-butyl)-4H-1-benzothiopyran-4-on-3-yl]-oxalic acid amide methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-amino-6-(n-butyl)-4H-1-benzothiopyran-4-one | HCID 20233128 | — |
| 反応物 | Oxalic acid monomethyl ester chloride | HCID 86640482 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | N-[6-(n-butyl)-4H-1-benzothiopyran-4-on-3-yl]-oxalic acid amide methyl ester | HCID 86741042 | — |
反応手順
2.94 g (0.024 mol) of oxalic acid monomethyl ester chloride are added to a solution of 5.05 g (0.0216 mol) of 3-amino-6-(n-butyl)-4H-1-benzothiopyran-4-one and 2.4 g (0.024 mol) of triethylamine in 325 ml of chloroform, the temperature of the reaction mixture rising to 30°. The mixture is then stirred for one hour at room temperature. The mixture is then concentrated to dryness by evaporation and the crystalline residue is stirred with ethanol, filtered with suction and washed first with ethanol and then with ether. After drying, N-[6-(n-butyl)-4H-1-benzothiopyran-4-on-3-yl]-oxalic acid amide methyl ester having a melting point of 192°-193.5° is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04614745 |
| 出典データセット | uspto-grants-1986_09 |
| ORD ID | ord-8f68ced42d6240b895461757e3233495 |
| 出典メモ | uspto-grants-1986_09 |