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Water → (S)-tert-Butyl (4-oxo-2,3,4,5-tetrahydrobenzo[b][1,4]oxazepin-3-yl)carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | (S)-3-(2-aminophenoxy)-2-((tert-butoxycarbonyl)amino)propanoic acid | HCID 18599735 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (S)-tert-Butyl (4-oxo-2,3,4,5-tetrahydrobenzo[b][1,4]oxazepin-3-yl)carbamate | HCID 18599719 | 87% |
反応手順
A mixture of (S)-3-(2-amino-phenoxy)-2-tert-butoxycarbonylamino-propionic acid (3.8 g, 12.8 mmol, 1 eq) and N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (EDCI, 2.46 g, 12.8 mmol, 1 eq) in DMF (56.4 mL) was stirred for 1 h 45 min. The reaction was poured into H2O (250 mL) and extracted with EtOAc. The combined extracts were washed with H2O, dried over Na2SO4 and concentrated to give the title compound (3.1 g, 87%) as a tan solid which was used without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09394263B2 |
| 出典データセット | uspto-grants-2016_07 |
| ORD ID | ord-1ca5891b47564a4a959e881e9b03746c |
| 出典メモ | uspto-grants-2016_07 |