Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium hydride → 3-[(6-Acetyl-2-chloro-pyridin-3-ylmethyl)-amino]-propionic acid tert-butyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | Tert-butyl 3-aminopropanoate hydrochloride | HCID 16218890 | — |
| 반응물 | Ethanone, 1-[5-(bromomethyl)-6-chloro-2-pyridinyl]- | HCID 86011816 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 3-[(6-Acetyl-2-chloro-pyridin-3-ylmethyl)-amino]-propionic acid tert-butyl ester | HCID 86595998 | — |
반응 단계
To a solution of 3-amino-propionic acid tert-butyl ester hydrochloride (1.5 eq) in DMF is added NaH (3.5 eq). The resulting mixture is stirred at room temperature for 15 minutes and a solution of 1-(5-bromomethyl-6-chloro-pyridin-2-yl)-ethanone (1 eq) in DMF is then added. After stirring for 3 hours, it is partitioned with 20% EtOAc/hexane and H2O. The organic layer is washed with brine and dried. After concentration, 3-[(6-acetyl-2-chloro-pyridin-3-ylmethyl)-amino]-propionic acid tert-butyl ester is isolated by flash column chromatography. MS: (ES+): 313.1 (M+1)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07939519B2 |
| 출처 데이터셋 | uspto-grants-2011_05 |
| ORD ID | ord-8792f304bc2f4e5180e35d4541450ba2 |
| 출처 메모 | uspto-grants-2011_05 |