Hydrochloric Acid → (+)-4-(3'-Methylpentanoyl)biphenyl

HRID 26336

Reaktionsgleichung

[C:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl-].[Cl-].[Cl-].[Al+3].[CH3:17][CH:18]([CH2:23][CH3:24])[CH2:19][C:20](Cl)=[O:21].Cl>[N+](C1C=CC=CC=1)([O-])=O.O>[CH3:17][CH:18]([CH2:23][CH3:24])[CH2:19][C:20]([C:4]1[CH:5]=[CH:6][C:1]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)=[CH:2][CH:3]=1)=[O:21]

Komponenten

Reaktionsbedingungen

Temperatur: -7 °C

Versuchsvorschrift

To commercially available biphenyl (0.08 mole) and anhydrous aluminium trichloride (0.1 mole) dissolved in dry nitrobenzene (90ml), (+)-3-methylpentanoylchloride (0.1mole) the preparation of which is known and described in United Kingdom Patent Application No. 36211/75), is added in drops, the temperature being maintained at about -7° C. during the addition. The mixture is then stirred for about 18 hr. with cooling in an ice bath. It is then poured onto a mixture of ice, water and concentrated hydrochloric acid and stirred for 0.5 hr., and the nitrobenzene layer is separated. The nitrobenzene is removed by steam distillation and the residue is crystallised from a small volume of ethanol to constant melting point.

Aufarbeitung

addition36211/75), is added in drops
temperaturewith cooling in an ice bath
stirringstirred for 0.5 hr
custom, and the nitrobenzene layer is separated
customThe nitrobenzene is removed by steam distillation
customthe residue is crystallised from a small volume of ethanol to constant melting point

Quellen und Nachweise

ORD-Eintrag: ord-d8bd9553888746338d44dceea6760389
Quelldatensatz: uspto-grants-1979_04
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04149413

Verknüpfte Notizen

Wird geladen…