Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → Rofecoxib
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | 2-(4-(Methylsulfonyl)phenyl)phenylacetylene | HCID 18400188 | — |
| 생성물 | Rofecoxib | HCID 5090 | — |
반응 단계
Into a 20 ml glass ampule are added 1 g of 2-(4-(methylsulfonyl)phenyl)phenylacetylene, 20 mg of Rh4 (CO)12, 1.5 g of Et3N, 10 ml of THF, 1 ml of water under nitrogen atmosphere, and the ampule is placed in a 100-ml stainless steel autoclave. The reaction system is flushed three times with CO then charged at room temperature to a initial CO pressure of 100 atm. The reaction is carried at 100° C. for 5 h. The solution is then diluted with 50 ml of benzene and washed with brine, 1N HCl. The benzene solution is dried over Na2SO4, and concentrated. The crude products are separated by column chromatography on silica gel eluted with 2:1 EtOAc/hexane to give the title compound and its regioisomer.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US05840746 |
| 출처 데이터셋 | uspto-grants-1998_11 |
| ORD ID | ord-4c61b74c0d1544e3994031dd0fcfd63b |
| 출처 메모 | uspto-grants-1998_11 |