Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diisopropylethylamine → Methyl 5-chloro-2-(2-phenylpyrrolidin-1-yl)nicotinate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 2-Phenylpyrrolidine | HCID 261892 | — |
| 반응물 | Methyl 2,5-Dichloronicotinate | HCID 2764318 | — |
| 용매 | Isopropanol | HCID 3776 | — |
| 생성물 | Methyl 5-chloro-2-(2-phenylpyrrolidin-1-yl)nicotinate | HCID 67958237 | 90.9% |
반응 단계
To a solution of Methyl 2,5-dichloronicotinate (120 mg, 0.58 mmol,) in isopropanol (10 ml), 2-phenylpyrrolidine (86 mg, 0.58 mmol, available from Matrix Scientific #018619) and N,N-Diisopropylethylamine (90 mg, 0.70 mmol) were added. The mixture was heated under reflux overnight. After cooling to room temperature, the mixture was evaporated and the residue was dissolved in ethyl acetate (10 ml), washed with water (10 ml) and brine (10 ml), dried over Na2SO4 and evaporated in vacuo. The crude residue was purified by flash chromatography on silica gel eluting with a mixture petroleum ether/ethyl acetate 20:1 to afford the title compound (D72) (167 mg) as colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08828987B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-5e3375791b904b1f97f0e2e9f6e535f8 |
| 출처 메모 | uspto-grants-2014_09 |