Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Benzenesulfonyl chloride, 2,4-dinitro- → HCID 86607837, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Benzenesulfonyl chloride, 2,4-dinitro- | HCID 74255 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | (S)-1-(3-bromophenyl)ethanamine | HCID 9952938 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | HCID 86607837 | HCID 86607837 | 94.4% |
반응 단계
To a stirred ice-cooled solution of (S)-(−)-3-bromo-α-methylbenzylamine (832 mg, 4.16 mmol, from Chiragene) in 15.6 mL of THF was added 1.33 g (4.99 mmol, 1.20 eq.) of 2,4-dinitrobenzenesulfonyl chloride, followed by 1.08 mL (6.20 mmol, 1.49 eq.) of N,N-diisopropylethylamine. The ice bath was removed, and the mixture was stirred at room temperature for 19 h and then concentrated. The residue was taken up in EtOAc, washed with 2×H2O, dried over Na2SO4, filtered, and concentrated. The residue was sonicated in ca. 5 mL of EtOAc until a precipitate was formed. The mixture was diluted to ca. 25 mL with hexanes. Filtration afforded product as a tan solid (1.69 g, 94.4% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07704995B2 |
| 출처 데이터셋 | uspto-grants-2010_04 |
| ORD ID | ord-04e21450f35d4604a32ae155474de354 |
| 출처 메모 | uspto-grants-2010_04 |