HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → 4'-(Hydroxymethyl)-2'-methylbiphenyl-2-carbonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | (4-Bromo-3-methylphenyl)methanol | HCID 10987288 | — |
| Reactant | 2-Cyano-phenylboric acid | HCID 21708089 | — |
| Catalyst | Tetrabutylammonium Bromide | HCID 74236 | — |
| Catalyst | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 4'-(Hydroxymethyl)-2'-methylbiphenyl-2-carbonitrile | HCID 67009731 | 24.5% |
Reaction Steps
A mixture of 4-bromo-3-methylbenzylalcohol (15.16 g), 2-cyanophenylboric acid (14.80 g), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II), dichloromethane adduct (3.08 g), tetrabutylammonium bromide (1.22 g), 2M aqueous sodium carbonate solution (75 mL) and toluene (300 mL) was refluxed under an argon atmosphere for 30 hr. The reaction mixture was concentrated, and the residue was dissolved in ethyl acetate. The obtained ethyl acetate solution was washed with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography to give the title compound as a pale-yellow oil (4.12 g, 24%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09115136B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-53b852d0b93344ba89960531664f335c |
| Source note | uspto-grants-2015_08 |