Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Carbonate → 5-(5,5-Dimethyl-4,5-dihydroisoxazol-3-ylsulfanylmethyl)-3-methoxy-isoxazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | Thiourea | HCID 2723790 | — |
| 반응물 | 5-(Bromomethyl)-3-methoxy-1,2-oxazole | HCID 10845405 | — |
| 반응물 | 3-Methylsulfonyl-5,5-dimethyl-2-isoxazoline | HCID 12137656 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 5-(5,5-Dimethyl-4,5-dihydroisoxazol-3-ylsulfanylmethyl)-3-methoxy-isoxazole | HCID 59739599 | 45% |
반응 단계
5-Bromomethyl-3-methoxy-isoxazole (1.22 g, 6.35 mmol) was dissolved in ethanol (30 ml) and thiourea (484 mg, 6.4 mmol) was added. The mixture was stirred at room temperature until the solids were dissolved. 3-Methanesulfonyl-5,5-dimethyl-4,5-dihydroisoxazole (1.08 g, 6.4 mmol) and potassium carbonate (880 mg, 6.4 mmol) were added and the mixture was heated under reflux for 1 hour. The solids were removed by filtration and the filtrate was concentrated. The crude product was purified by chromatography on silica gel (eluent: ethyl acetate/hexane) to give the product as colourless oil (0.69 g, 45% yield over 3 steps).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08680290B2 |
| 출처 데이터셋 | uspto-grants-2014_03 |
| ORD ID | ord-1b84df4719be4e77bd721b89be15f453 |
| 출처 메모 | uspto-grants-2014_03 |