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Diethyl Ether → Ethyl N-(thiophene-2-carbonyl)glycinate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Thiophenecarbonyl chloride | HCID 78928 | — |
| 反応物 | Glycine ethyl ester, hydrochloride | HCID 2723640 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Ethyl N-(thiophene-2-carbonyl)glycinate | HCID 1720748 | 68.4% |
反応手順
To a solution of glycine ethyl ester hydrochloride (22 g) and potassium carbonate (86 g) in water (600 ml) was added a mixture of benzene (600 ml) and ether (400 ml) and stirred at room temperature. 2-Thenoyl chloride (25 g) in benzene (100 ml) was added during a period of about 30 minutes under stirring and then the mixture was stirred for 2 hours at room temperature. The organic layer was separated and after dried over anhydrous sodium sulfate, concentrated under reduced pressure to give colorless crystals, which were recrystallized from ethanol to obtain the objective compound (23 g), mp 82°-83° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04914104 |
| 出典データセット | uspto-grants-1990_04 |
| ORD ID | ord-d8668908c7e54640b4194c55a0f5fa75 |
| 出典メモ | uspto-grants-1990_04 |