Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diethyl Oxalate → 3-(2-Nitro-3-piperidin-1-yl-phenyl)-2-oxo-propionic acid ethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diethyl Oxalate | HCID 7268 | — |
| 반응물 | Lithium diisopropylamide | HCID 2724682 | — |
| 반응물 | (4-(4-Methylpiperidin-1-yl)-3-nitrophenyl)methanol | HCID 28963353 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 3-(2-Nitro-3-piperidin-1-yl-phenyl)-2-oxo-propionic acid ethyl ester | HCID 59796771 | — |
반응 단계
A solution of 1-(3-methyl-2-nitro-phenyl)-piperidine (i) in THF is treated with lithium diisopropylamide (“LDA”) (1 eq), followed by diethyl oxalate (1.05 eq), at 0° C. The reaction is allowed to warm to room temperature over 90 min. The reaction is diluted with water and ether, partitioned, and the aqueous layer is washed with ether. The combined organic layers are dried over MgSO4, filtered and concentrated. Chromatography gives 3-(2-nitro-3-piperidin-1-yl-phenyl)-2-oxo-propionic acid ethyl ester (ii).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07790724B2 |
| 출처 데이터셋 | uspto-grants-2010_09 |
| ORD ID | ord-5b64d57edf6740d3b81f185e2a7dd28d |
| 출처 메모 | uspto-grants-2010_09 |