HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethanolamine → Benzenemethanol, 2,4-dichloro-α-methyl-, (αR)-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethanolamine | HCID 8113 | — |
| Reactant | 2',4'-Dichloroacetophenone | HCID 16693 | — |
| Reactant | Chlorobis((1S,2R,3S,5S)-2,6,6-trimethylbicyclo(3.1.1)hept-3-yl)borane | HCID 9923113 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Benzenemethanol, 2,4-dichloro-α-methyl-, (αR)- | HCID 6950773 | 82.2% |
Reaction Conditions
| Temperature | -25 °C |
|---|
Reaction Steps
To a solution of 2′,4′-dichloroacetophenone (10.9 g, 77.0 mmol) in anhydrous THF (80 mL) at −78° C. under nitrogen was slowly added a solution of (+)-B-chlorodiisopinocampheylborane ((+)-Ipc2BCl, 27.2, 85.0 mmol) in THF (15 mL). After the addition is complete, the reaction mixture was slowly warmed to −25° C. and stirred at this temperature for 2 h. The reaction mixture was then quenched with diethanolamine (17.9 g, 170 mmol), and stirred for 10 min. During this time, a solid formed and it was filtered off. The filtrate was dried (Na2SO4), filtered, and concentrated in vacuo. The residue was purified flash chromatography (SiO2, 0-20% ethyl acetate in hexanes) to give (R)-1-(2,4-dichlorophenyl)ethanol (12.0 g, 63.3 mmol, 82%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09150550B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-ffd2d039cac04743b9244457ae475701 |
| Source note | uspto-grants-2015_10 |