Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → (+/-)-Ethyl 4-[4-(benzyloxy)phenyl]-2-methyl-2-(methylsulfonyl)butanoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | Ethyl 4-[4-(benzyloxy)phenyl]-2-(methylsulfonyl)butanoate | HCID 66577987 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | (+/-)-Ethyl 4-[4-(benzyloxy)phenyl]-2-methyl-2-(methylsulfonyl)butanoate | HCID 56951003 | 91% |
반응 단계
Cesium carbonate (9.30 g, 28.5 mmol) was added to ethyl 4-[4-(benzyloxy)phenyl]-2-(methylsulfonyl)butanoate (8.86 g, 23.5 mmol) in DMF (100 mL) and stirred for 30 minutes. Iodomethane was added to the reaction followed by stirring overnight at room temperature. The reaction mixture was poured into 1N aqueous HCl (100 mL) and extracted with EtOAc (3×100 mL). The combined organics were washed with saturated aqueous sodium thiosulfate (100 mL) then dried (MgSO4), filtered and concentrated in vacuo to afford a crude solid. The crude product was purified via silica gel chromatography using an eluant of ethyl acetate in heptane (10-100%) to afford the title compound as a white solid (8.35 g, 90.9%). LC-MS m/z 391.2 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08853258B2 |
| 출처 데이터셋 | uspto-grants-2014_10 |
| ORD ID | ord-ae2ebe9007594ae39d0c62eb5b266e55 |
| 출처 메모 | uspto-grants-2014_10 |