Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium Hydroxide → 3,5-Bis(4-bromophenyl)isoxazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 1,3-Propanedione, 1,3-bis(4-bromophenyl)- | HCID 147438 | — |
| 반응물 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 3,5-Bis(4-bromophenyl)isoxazole | HCID 12207756 | — |
반응 단계
In a 250 ml round bottom flask, 4 g (10.4 mmol) of [2] was dissolved in 100 ml dry dioxane and heated to reflux, then 3.0 g (43.2 mmol) hydroxylamine hydrogen chloride in 10 ml water and 5 ml (25 mmol) 5 N NaOH was then dropped into the refluxing mixture. After 12 hours, the reaction mixture was cooled down to room temperature, and the solvent was removed in vacuo. The product was recrystallized from ethanol. Characterization. Yield: 3.41 g (85%). M.P. 218.5–219.5° C. 1HNMR (300 MHz, CDCl3, 20° C., δ); 7.78 (d, 2H, ArH), 7.74 (d, 2H, Ar′H), 7.66 (d, 2H, ArH), 7.62 (d, 2H, Ar′H), 6.82 (s, 1H, isoxazole proton). EI-MS: 379 (M+), 224, 183, 155.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07094121B2 |
| 출처 데이터셋 | uspto-grants-2006_08 |
| ORD ID | ord-0adf17f674044210915e55a9d072a99b |
| 출처 메모 | uspto-grants-2006_08 |