Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Aniline → 1-(4-(Naphthalen-2-ylsulfonyl)piperazin-1-yl)-2-(phenylamino)ethanone
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Aniline | HCID 6115 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | 2-Chloro-1-[4-(naphthalene-2-sulfonyl)piperazin-1-yl]ethan-1-one | HCID 2405875 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 1-(4-(Naphthalen-2-ylsulfonyl)piperazin-1-yl)-2-(phenylamino)ethanone | HCID 67980417 | 86.2% |
반응 단계
A stirred solution of aniline (15.3 g, 0.16 mol) and di-isopropyl ethylamine (DIEA, 56 mL, 0.33 mol) in acetonitrile (120 mL) is heated to 60° C. and 2-chloro-1-(4-(naphthalen-2-ylsulfonyl)piperazin-1-yl)ethanone (compound 5, 0.3 g, 0.85 mmol) is added dropwise. The reaction mixture is kept stirring at this temperature for another 3 h and is then evaporated to dryness. Water is added to the residue, and extracted with ethyl acetate (2×30 mL). The organic extract was dried over anhydrous sodium sulphate, filtered and concentrated under reduced pressure. The resultant crude product was purified by column chromatography on silica gel (hexane:ethyl acetate:3:7) to obtain the title compound (300 mg, 76.53%) as an off-white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09115086B2 |
| 출처 데이터셋 | uspto-grants-2015_08 |
| ORD ID | ord-026d16cb4369425b8cedeed47607e5c2 |
| 출처 메모 | uspto-grants-2015_08 |