Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Carbonate → N,N-bis(3-methylbutyl)-4-nitro-3-[(3-piperidin-1-ylpropyl)amino]benzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Piperidine-1-propylamine | HCID 19049 | — |
| 반응물 | 3-fluoro-N,N-bis(3-methylbutyl)-4-nitrobenzamide | HCID 68447111 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | N,N-bis(3-methylbutyl)-4-nitro-3-[(3-piperidin-1-ylpropyl)amino]benzamide | HCID 68446148 | 78% |
반응 단계
A mixture of 3-fluoro-N,N-bis(3-methylbutyl)-4-nitrobenzamide (430 mg, 1 eq, prepared according to Example A1), 3-piperidino-propylamine (212 mg, 1.1 eq) and potassium carbonate (365 mg, 2 eq) in acetonitrile (10 ml) is heated under reflux for 3 hours then concentrated under reduced pressure at 40° C. The residue is taken up in dichloromethane (50 ml) and water (20 ml). After decantation and extractions, the combined organic phases are washed with salt water, dried over Na2SO4 then concentrated under reduced pressure at 40° C. Purification of the residue by flash chromatography on silica gel (eluent: ethyl acetate 100%) produces the expected compound in the form of a yellow oil (460 mg; 78% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07355052B2 |
| 출처 데이터셋 | uspto-grants-2008_04 |
| ORD ID | ord-7648f6e127604772a5e58a726f575ffd |
| 출처 메모 | uspto-grants-2008_04 |