Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanesulfonic Acid → (3R)-3-(2,6-Dichloro-4-hydroxy-benzyl)-1-(4,5,6,7-tetrahydro-1H-indazol-7-yl)-pyrrolidin-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanesulfonic Acid | HCID 6395 | — |
| 반응물 | (R)-3-(4-benzyloxy-2,6-dichloro-benzyl)-1-(4,5,6,7-tetrahydro-1H-indazol-7-yl)-pyrrolidin-2-one | HCID 67316393 | — |
| 용매 | Dimethyl Sulfide | HCID 1068 | — |
| 생성물 | (3R)-3-(2,6-Dichloro-4-hydroxy-benzyl)-1-(4,5,6,7-tetrahydro-1H-indazol-7-yl)-pyrrolidin-2-one | HCID 67316404 | 110.6% |
반응 단계
To a solution of (R)-3-(4-benzyloxy-2,6-dichloro-benzyl)-1-(4,5,6,7-tetrahydro-1H-indazol-7-yl)-pyrrolidin-2-one (2.46 g, 5.23 mmol) in dimethylsulfide (28 mL), add methane sulfonic acid (8.23 g, 85.7 mmol) and stir the mixture vigorously under at room temperature for 18 hours. Remove the solvent in vacuo and dilute the residue with water, adjust the pH to pH=7 with 5 N NaOH, and extract the mixture several times with ethyl acetate and THF. After drying the combined organic layer (Na2SO4), filter and concentrate under vacuum to afford 2.20 g (100%) of the title compound. MS (m/z): 381 (M+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07981918B2 |
| 출처 데이터셋 | uspto-grants-2011_07 |
| ORD ID | ord-18d1d8da0f5f4e8d83285295930e5853 |
| 출처 메모 | uspto-grants-2011_07 |