Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Tetrahydrofuran → 4-Methoxy-2-(2-methyl-[1,3]-dioxolan-2-yl)benzoxazole-7-carboxylic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 1,3-Bis(diphenylphosphino)propane | HCID 81219 | — |
| 반응물 | 7-Bromo-4-methoxy-2-(2-methyl-[1,3]-dioxolan-2-yl)benzoxazole | HCID 18316652 | — |
| 반응물 | HCID 178418416 | HCID 178418416 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 4-Methoxy-2-(2-methyl-[1,3]-dioxolan-2-yl)benzoxazole-7-carboxylic acid | HCID 18316634 | — |
반응 단계
7-Bromo-4-methoxy-2-(2-methyl-[1,3]-dioxolan-2-yl)benzoxazole (480 mg), palladium acetate (34 mg), 1,3-bis(diphenylphosphino)propane (126 mg), triethylamine (0.21 ml), water (15 ml) and tetrahydrofuran (30 ml) were combined and heated to 90° C. in a Parr apparatus under 1035 kPa (150 psi) of carbon monoxide for 3 days. After cooling to room temperature, the tetrahydrofuran was evaporated in vacuo. The residue was partitioned between ethyl acetate (50 ml) and water (50 ml). The aqueous layer was extracted with ethyl acetate (50 ml). The combined organic extracts were dried over magnesium sulphate, evaporated in vacuo and purified by flash chromatography eluting with ethyl acetate to yield the title compound as a white solid (190 mg).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06353010B1 |
| 출처 데이터셋 | uspto-grants-2002_03 |
| ORD ID | ord-c26c330d25cb49308191857aa8d3dfd8 |
| 출처 메모 | uspto-grants-2002_03 |