Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2-Dimethylaminopyridine → 2,3-Dihydro-1h-inden-2-yl methanesulfonate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2-Dimethylaminopyridine | HCID 21885 | — |
| 반응물 | Methanesulfonyl chloride | HCID 31297 | — |
| 반응물 | 2-Indanol | HCID 77936 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2,3-Dihydro-1h-inden-2-yl methanesulfonate | HCID 255221 | 78% |
반응 단계
2-Indanol (20.00 g, 149.5 mmol) and diisopropylethylamine (21.2 g, 164 mmol) was stirred in dichloromethane (300 mL) at 0° C. Methanesulfonyl chloride (18.78 g, 164 mmol) and dimethylaminopyridine (1.80 g) were added simultaneously and stirring continued at room temperature for 18 h. Solution was evaporated, partitioned between ethyl acetate and water, and the organic phase separated. This was washed with NaHCO3 (sat) and with citric acid solution (5%) and dried over MgSO4. The filtered solution was concentrated and the resultant solid recrystallized from isopropanol-EtOH (3:1) to give off-white crystals (24.6 g, 78%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08486984B2 |
| 출처 데이터셋 | uspto-grants-2013_07 |
| ORD ID | ord-8a773c1aeae7433abb88a6f5b83d4413 |
| 출처 메모 | uspto-grants-2013_07 |