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(Tert-butoxycarbonyl)aspartic acid → 3-(Boc-amino)dihydrofuran-2,5-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | (Tert-butoxycarbonyl)aspartic acid | HCID 302432 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-(Boc-amino)dihydrofuran-2,5-dione | HCID 3757779 | — |
反応手順
A mixture of 1 g (4.29 mmol) of N-(tert-butoxycarbonyl)-DL-aspartic acid and 0.98 g (5.15 mmol) of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDCI) in 100 mL of DCM, was stirred at room temperature overnight. The solution was extracted three times with 5% aq. NaHSO4, the organic extracts were dried over anh. sodium sulfate and the solvent evaporated under vacuum. In this way 750 mg of the title compound were recovered. 1H NMR (400 MHz, DMSO-D6) δ ppm 1.38 (s, 9 H) 2.78-2.90 (m, 1 H) 3.15-3.28 (m, 1 H) 4.54-4.65 (m, 1 H) 7.73 (d, J=7.91 Hz, 1 H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07618982B2 |
| 出典データセット | uspto-grants-2009_11 |
| ORD ID | ord-441468b8f1794221b684e37447bc2130 |
| 出典メモ | uspto-grants-2009_11 |