Menthol → Dichloro((1R,2S,5R)-2-isopropyl-5-methylcyclohexyloxy)phosphine

HRID 41825

Reaktionsgleichung

[P:1]([Cl:4])(Cl)[Cl:2].[CH:5]1([CH3:15])[CH2:10][CH2:9][CH:8]([CH:11]([CH3:13])[CH3:12])[CH:7]([OH:14])[CH2:6]1>ClCCl>[Cl:2][P:1]([Cl:4])[O:14][C@@H:7]1[CH2:6][C@H:5]([CH3:15])[CH2:10][CH2:9][C@H:8]1[CH:11]([CH3:13])[CH3:12]

Komponenten

Reaktionsbedingungen

Temperatur: -30 °C

Versuchsvorschrift

The phosphorus trichloride (56.0 ml, 87.89 g, 0.640 mol) was added to dichloromethane (anhydrous) under argon gas to obtain a solution. The solution was cooled to −30° C. and (−)-menthol (1R,2S,5R) (10.00 g, 0.0640 mol) was added portion wise over 10 mins. The solution was allowed to warm to ambient temperature and was allowed to stir at ambient temperature for 16 hours. The solvent was removed in vacuo to obtain a colourless oil (16.46 g). The crude product was used directly in the subsequent step.

Aufarbeitung

customto obtain a solution
temperatureto warm to ambient temperature
customThe solvent was removed in vacuo

Quellen und Nachweise

ORD-Eintrag: ord-418ec2ccf0174a49964151744e04de0f
Quelldatensatz: uspto-grants-2013_09
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US08535655B2

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