Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2-(dimethylamino)-4-(trifluoromethyl)-6H-1,3-oxazin-6-one → 3-(6-Fluoro-3-methyl-1,2-benzisoxazol-5-yl)-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2-(dimethylamino)-4-(trifluoromethyl)-6H-1,3-oxazin-6-one | HCID 3723862 | — |
| 반응물 | 6-Fluoro-3-methylbenzo[d]isoxazol-5-amine | HCID 18314470 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 3-(6-Fluoro-3-methyl-1,2-benzisoxazol-5-yl)-6-(trifluoromethyl)-2,4(1H,3H)-pyrimidinedione | HCID 18314502 | 73.3% |
반응 단계
A mixture of 5-amino-6-fluoro-3-methyl-1,2-benzisoxazole (4.85 g, 0.029 mol) and 2-dimethylamino-4-(trifluoromethyl)-6H-1,3-oxazin-6-one (6.70 g, 0.0320 mol) in acetic acid is refluxed for 90 minutes, cooled to room temperature, and poured into an ice-water mixture. The resultant aqueous mixture is filtered to obtain a solid. The solid is air-dried and dissolved in ethyl acetate. The resultant organic solution is washed with brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to give the title product as a yellow solid (7.00 g, mp 235-237° C.) which is identified by NMR spectral analyses.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06355796B1 |
| 출처 데이터셋 | uspto-grants-2002_03 |
| ORD ID | ord-4ce46596b9ed4e759054c3cee9135dc7 |
| 출처 메모 | uspto-grants-2002_03 |