Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
2-Isopropoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolane → 2-[2-(Cyclopropylmethoxy)-5-(difluoromethyl)phenyl]-4,4,5,5-tetramethyl-1,3,2-dioxaborolane
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 2-Isopropoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolane | HCID 5017741 | — |
| 반응물 | 2-Bromo-1-(cyclopropylmethoxy)-4-(difluoromethyl)benzene | HCID 67033012 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Butyl methyl ether | HCID 12338 | — |
| 생성물 | 2-[2-(Cyclopropylmethoxy)-5-(difluoromethyl)phenyl]-4,4,5,5-tetramethyl-1,3,2-dioxaborolane | HCID 67033178 | 98.6% |
반응 단계
2-Bromo-1-cyclopropylmethoxy-4-difluoromethyl-benzene (example B.b18; 24.35 g; 87.9 mmol) is dissolved in dry tert. BuOMe (440 mL). n-BuLi (1.6M in hexane; 60.0 mL; 96.0 mmol) is slowly syringed into the well stirred reaction mixture at −40° C. After one hour commercially available 2-isopropoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (17.86 g; 96.0 mmol) is added at −40° C. followed by stirring at 0° C. for one additional hour. The reaction mixture is quenched by addition of 2M aqueous citric acid (90.0 mL). The organic layer is separated, washed with brine, dried over Mg2SO4 and filtered through a pad of neutral alumina (act.2-3). The solvent is removed under reduced pressure to yield 28.1 g of the title compound as pale yellow oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US09376442B2 |
| 출처 데이터셋 | uspto-grants-2016_06 |
| ORD ID | ord-7c89ceca2fd849fabc2619d1b5447c09 |
| 출처 메모 | uspto-grants-2016_06 |