참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 2,2,2-Trifluoroethyl trifluoromethanesulfonate | HCID 80366 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | 5-bromo-2,3-dihydro-1H-isoindol-1-one | HCID 22607119 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 5-Bromo-2-(2,2,2-trifluoroethyl)-2,3-dihydro-1H-isoindol-1-one | HCID 59420755 | — |
반응 단계
5-Bromo-2,3-dihydro-1H-isoindol-1-one (100 mg, 0.47 mmol) was dissolved in DMF (4.7 mL) and stirred at 0° C. NaH (38 mg, 0.94 mmol, 60% dispersion in oil) was carefully added in two portions, and the resulting mixture was allowed to stir at 0° C. for 15 minutes before 2,2,2-trifluoroethyl trifluoromethanesulfonate (110 mg, 0.47 mmol) was added. The mixture was allowed to stir at 0° C. for 30 minutes before saturated aqueous NaHCO3 (10 mL) was carefully added, and the mixture was extracted with EtOAc. The organic layer was washed with water, brine, dried over anhydrous MgSO4, filtered, and concentrated in vacuo. The residue was purified by MPLC on silica gel (using a gradient elution of 0-20% EtOAc/hexanes). Desired fractions were identified, combined, and concentrated in vacuo to afford the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09328099B2 |
|---|
| 출처 데이터셋 | uspto-grants-2016_05 |
|---|
| ORD ID | ord-e699ce3aae414cb883005f3676016e85 |
|---|
| 출처 메모 | uspto-grants-2016_05 |
|---|