HuagongsheHuagongshe Chemistry Print Report · For research reference only
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
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Isopropoxy-4,4,5,5-tetramethyl-1,3,2-dioxaborolane | HCID 5017741 | — |
| Reactant | 2-Bromo-1-(cyclopropylmethoxy)-4-(difluoromethyl)benzene | HCID 67033012 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Solvent | Butyl methyl ether | HCID 12338 | — |
| Product | 2-[2-(Cyclopropylmethoxy)-5-(difluoromethyl)phenyl]-4,4,5,5-tetramethyl-1,3,2-dioxaborolane | HCID 67033178 | 98.6% |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09376442B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-7c89ceca2fd849fabc2619d1b5447c09 |
| Source note | uspto-grants-2016_06 |