참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 반응물 | 1-Hydroxybenzotriazole hydrate | HCID 2796029 | — |
| 반응물 | (S)-Boc-Diaminobutyric acid | HCID 86752309 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | (S)-tert-Butyl (2-oxopyrrolidin-3-yl)carbamate | HCID 10750535 | 85.2% |
반응 단계
(S)-Boc-Diaminobutyric acid (25 g, 115 mmol), triethylamine (35 g, 344 mmol), and 1-hydroxybenzotriazole hydrate (19.3 g, 143 mmol) are dissolved in 300 mL of THF. 1-(3-Dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (27.4 g, 143 mmol) is added to the solution. The solution is heated at 60° C. over 15 min. A white precipitate forms and the solution is kept at 60° C. for 4 h. After this time, the solution is filtered and the collected liquid is concentrated. The crude product is purified by column chromatography eluting with a gradient of 1% MeOH/CH2Cl2 to 3% MeOH/CH2Cl2 to afford the title compound (19.6 g, 98 mmol) as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05731315 |
|---|
| 출처 데이터셋 | uspto-grants-1998_03 |
|---|
| ORD ID | ord-0a8a7f7391de4560854070e9af7b0eeb |
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| 출처 메모 | uspto-grants-1998_03 |
|---|
