Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → HCID 178434636, 화합물
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Hydrazine, dihydrochloride | HCID 17548 | — |
| 반응물 | 2-(8-Fluoro-2,3-dihydro-1,4-benzodioxin-6-yl)-3-oxobutanenitrile | HCID 66891603 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | HCID 178434636 | HCID 178434636 | 93% |
반응 단계
2-(8-fluoro-2,3-dihydro-1,4-benzodioxin-6-yl)-3-oxobutanenitrile (0.37 g; 1.56 mmol) was dissolved in dry ethanol (5 mL) and hydrazine dihydrochloride (0.20 g, 1.87 mmol) then triethylamine (217 μg, 1.56 mmol) were added. The reaction mixture was refluxed for 2 h, cooled to rt and the solvent was evaporated under vacuum. The residue was dissolved in ethyl acetate (50 ml), washed with saturated sodium bicarbonate (2×25 mL), brine (25 ml) then dried over sodium sulfate. Filtration and concentration gave 4-(8-fluoro-2,3-dihydro-1,4-benzodioxin-6-yl)-3-methyl-1H-pyrazol-5-amine (0.36 g, 93% yield) as an orange solid. 1H NMR (400 MHz, d6-DMSO) δ 6.75 (dd, 1H), 6.65 (m, 1H), 4.30 (m, 4H), 2.14 (s, 3H). MS (EI) for C12H12FN3O2: 250 (MH+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07872014B2 |
| 출처 데이터셋 | uspto-grants-2011_01 |
| ORD ID | ord-2ab85eabb79246c9b87bc937062b31b8 |
| 출처 메모 | uspto-grants-2011_01 |