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Isopropylsulphamoyl chloride → Methyl 2-((((1-methylethyl)amino)sulfonyl)amino)-3-pyridine carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Isopropylsulphamoyl chloride | HCID 117737 | — |
| 反応物 | Methyl 2-aminopyridine-3-carboxylate | HCID 351633 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 生成物 | Methyl 2-((((1-methylethyl)amino)sulfonyl)amino)-3-pyridine carboxylate | HCID 13609242 | — |
反応手順
Methyl 2-amino-3-pyridine carboxylate (10.0 grams; 0.066 mole) and isopropyl sulfamoyl chloride (11.4 grams; 0.066 mole) were mixed with 300 ml of benzene and the resulting reaction mixture heated at reflux temperatures for a period of 48 hours. Following the reaction period, the reaction mixture was cooled and the solvent removed in vacuo. The oily residue thus obtained was extracted with 200 ml of cyclohexane and the extracts combined and cooled. The resulting precipitate was recovered by filtration and recrystallized from carbon tetrachloride. As a result of these operations, the desired title compound having a melting point of 121° C.-123° C. was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04129734 |
| 出典データセット | uspto-grants-1978_12 |
| ORD ID | ord-d751186db3c44b318877fb3211ccbabf |
| 出典メモ | uspto-grants-1978_12 |