Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ammonia → Sulfonium, triphenyl-, 7,7-dimethyl-2-oxobicyclo[2.2.1]heptane-1-methanesulfonate (1:1)
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Bicyclo[2.2.1]heptane-1-methanesulfonic acid, 7,7-dimethyl-2-oxo-, (1S)- | HCID 18462 | — |
| 반응물 | Triphenylsulfonium iodide | HCID 21881071 | — |
| 반응물 | Ethyl ortho-acetate | HCID 86598186 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Sulfonium, triphenyl-, 7,7-dimethyl-2-oxobicyclo[2.2.1]heptane-1-methanesulfonate (1:1) | HCID 21930749 | 82.9% |
반응 단계
Triphenylsulfonium iodide (390 mg; 1 mmol), ethyl orthoacetate (486 mg; 3 mmol), and camphorsulfonic acid (278 mg; 1.2 mmol) were dissolved in anhydrous methylene chloride (10 ml), and the resultant mixture was stirred for 12 hours at room temperature. The reaction mixture was alkalinized by adding 1% aqueous ammonia (10 ml), and subjected to extraction with methylene chloride three times, followed by drying. The solvent was removed through distillation, and the thus-obtained semi-solid matter was washed with ether, to thereby yield 410 mg of the target compound as white crystals (yield: 82%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07335787B2 |
| 출처 데이터셋 | uspto-grants-2008_02 |
| ORD ID | ord-9a0b16546fde441eaa5969d3b43d34e2 |
| 출처 메모 | uspto-grants-2008_02 |