참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 4-Methylmorpholine | HCID 7972 | — |
| 반응물 | 2-Dimethylaminopyridine | HCID 21885 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 반응물 | N-Boc-L-Leucine Hydrate | HCID 12373896 | — |
| 반응물 | methyl (5R)-5-((trimethylsilyl)ethynyl)-L-prolinate | HCID 16090847 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 66757129 | HCID 66757129 | — |
반응 단계
To a solution of methyl (5R)-5-((trimethylsilyl)ethynyl)-L-prolinate (1.6 grams, 7.48 mmol), dimethylaminopyridine (913 mg, 7.48 mmol), N-methylmorpholine (1.23 mL, 11.22 mmol), and N-(tert-butoxycabonyl)-L-leucine monohydrate (2.24 g, 8.98 mmol) in dichloromethane (30 mL) at room temperature was added 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (1.72 g, 8.98 mmol). The resulting mixture was stirred 16 hours at room temperature, and partitioned between ethyl acetate (200 mL) and 1 MHO (200 mL). The aqueous layer was further extracted with ethyl acetate (200 mL). The combined organic layers were dried (sodium sulfate), filtered, and concentrated. The residue was chromatographed with a Biotage 40 M cartridge with 40% ethyl acetate/hexane provide the titled compound. MS (DCI/NH3) m/e 439 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08637546B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_01 |
|---|
| ORD ID | ord-c31bfe24068f42b18859e38709bc86ef |
|---|
| 출처 메모 | uspto-grants-2014_01 |
|---|
