Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methanol → (R)-N-(4,4-Difluorocyclohexyl)-1-(4-(trifluoromethyl)phenyl)-3,4-dihydroisoquinoline-2(1H)-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | (R)-1-(4-(trifluoromethyl)phenyl)-1,2,3,4-tetrahydroisoquinoline | HCID 28293305 | — |
| 반응물 | HCID 59536363 | HCID 59536363 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | (R)-N-(4,4-Difluorocyclohexyl)-1-(4-(trifluoromethyl)phenyl)-3,4-dihydroisoquinoline-2(1H)-carboxamide | HCID 59536316 | — |
반응 단계
To a solution of (R)-1-(4-(trifluoromethyl)phenyl)-1,2,3,4-tetrahydroisoquinoline (80 mg, 0.29 mmol) in MeCN (2 mL) was added 4-nitrophenyl 4,4-difluoro-cyclohexylcarbamate (217 mg, 0.72 mmol). The resulting mixture was then subjected to microwave irradiation at 120° C. for 15 min. Then, MeOH (0.5 mL) was added and the mixture was filtered. The filtrate was purified by preparative HPLC (0%-100% MeCN 0.1% TFA/H2O 0.1% TFA) to give the title compound, which was dissolved in MeOH (1 mL). The solution was then passed through PL-HCO3 and the resin was washed with MeOH (2×0.3 mL). The combined filtrates were concentrated and dried in vacuo to give the title compound as a light-yellow solid. MS (ESI, positive ion) m/z: 439 (M+H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08476297B2 |
| 출처 데이터셋 | uspto-grants-2013_07 |
| ORD ID | ord-f8b4985b3b3749aabaadeb4cf7bc08a5 |
| 출처 메모 | uspto-grants-2013_07 |