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Water → 3-Carbomethoxy-4-[(chloroacetyl)amino]thiophene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Chloroacetyl chloride | HCID 6577 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methyl 4-aminothiophene-3-carboxylate Hydrochloride | HCID 2777609 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Carbomethoxy-4-[(chloroacetyl)amino]thiophene | HCID 14510003 | — |
反応手順
A suspension of 12.2 g (0.063 mol) of 3-carbomethoxy-4-aminothiophene hydrochloride in 100 ml of methylene chloride is treated with 10 ml (0.126 mol) of chloroacetyl chloride and subsequently dropwise with 17.6 ml (0.126 mol) of triethylamine, the temperature being held below 25° C. The solution is poured into water and extracted twice with 50 ml of methylene chloride each time. The combined methylene chloride extracts are washed three times with 50 ml of water each time, dried over magnesium sulphate and evaporated. After chromatography on silica gel using methylene chloride for the elution, there is obtained crystalline 3-carbomethoxy-4-[(chloroacetyl)amino]thiophene of melting point 98°-100° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04346030 |
| 出典データセット | uspto-grants-1982_08 |
| ORD ID | ord-921ea17b577148dfb7770cb6369f2f1f |
| 出典メモ | uspto-grants-1982_08 |