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Potassium Carbonate → ethyl 3-[N,N'-bis(tert-butyloxycarbonyl)hydrazino]-2,5-dioxopyrrolidine-3-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Di-tert-butyl azodicarboxylate | HCID 97268 | — |
| 反応物 | Ethyl 2,5-dioxo-3-pyrrolidinecarboxylate | HCID 23635561 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | ethyl 3-[N,N'-bis(tert-butyloxycarbonyl)hydrazino]-2,5-dioxopyrrolidine-3-carboxylate | HCID 67342586 | 83.1% |
反応手順
To a solution of ethyl 2,5-dioxopyrrolidine-3-carboxylate (2.96 g) in ethyl acetate (25 ml) were added di-tert-butyl azodicarboxylate (4.19 g) and then potassium carbonate (4.78 g) at room temperature. After this reaction mixture was stirred at room temperature for 15 minutes, the resulting mixture was filtered through a Celite pad and the filtrate was concentrated. The residue was purified by a flash column chromatography (hexane:ethyl acetate=3:1) to give ethyl 3-[N,N′-bis(tert-butyloxycarbonyl)hydrazino]-2,5-dioxopyrrolidine-3-carboxy late (5.77 g, 83%) as amorphous.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08058456B2 |
| 出典データセット | uspto-grants-2011_11 |
| ORD ID | ord-1079f7c1cd5d4a2db7acc72a56001f20 |
| 出典メモ | uspto-grants-2011_11 |