참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Cyclobutanone | HCID 14496 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | 3,4-Difluoroanisole | HCID 568250 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-(2,3-Difluoro-6-methoxyphenyl)-1-cyclobutanol | HCID 58022066 | 88% |
반응 단계
To a solution of 3,4-difluoroanisole (2.47 g) in tetrahydrofuran (50 mL) was added n-butyllithium (2.64 mol/L n-hexane solution, 6.5 mL) at −78° C., and the mixture was stirred at the same temperature for 30 minutes. To the reaction mixture was added a solution of cyclobutanone (1 g) in tetrahydrofuran (20 mL), and the mixture was stirred at the same temperature for 30 minutes. To the reaction mixture was added a saturated aqueous ammonium chloride solution, and the resulting mixture was extracted with diethyl ether. The extract was washed with water and brine successively, and dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure, and the residue was purified by column chromatography on silica gel (eluent: n-hexane/ethyl acetate=5/1) to give the title compound (2.69 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09040693B2 |
|---|
| 출처 데이터셋 | uspto-grants-2015_05 |
|---|
| ORD ID | ord-45f06d753e55429f876bd61caeebbfe9 |
|---|
| 출처 메모 | uspto-grants-2015_05 |
|---|