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1-Hydroxybenzotriazole → (S)-t-Butyl 2-(2-(2-(3,4-dimethoxyphenoxy)acetyl)hydrazinecarbonyl)pyrrolidine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | tert-Butyl (2S)-2-(hydrazinecarbonyl)pyrrolidine-1-carboxylate | HCID 10014050 | — |
| 反応物 | HCID 21835839 | HCID 21835839 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | (S)-t-Butyl 2-(2-(2-(3,4-dimethoxyphenoxy)acetyl)hydrazinecarbonyl)pyrrolidine-1-carboxylate | HCID 86706750 | 66.1% |
反応手順
To a solution of (S)-t-butyl 2-(hydrazinecarbonyl)pyrrolidine-1-carboxylate (50.0 g) and 2-(3,4-dimethoxyphenoxy)acetic acid (47.8 g) in chloroform (1000 ml), HOBt (35.3 g) and WSC hydrochloride (50.0 g) were added and the mixture was stirred at room temperature for 4 hours. After distilling off the solvent under reduced pressure, water was added, followed by extraction with ethyl acetate. The organic layer was washed successively with saturated aqueous sodium bicarbonate and brine and dried over MgSO4 before it was filtered. The solvent was distilled off under reduced pressure to give a crude form of the titled compound (61.0 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09181229B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-f0563710e9da4890b82dcb6b60a8fa9f |
| 出典メモ | uspto-grants-2015_11 |