Reaktion #467251

Reaktionsgleichung

methanol

diphenylphosphine

potassium

sodium 2-(2-fluorophenyl)glycinate

→

2-diphenylphosphino-α-phenylglycine

Lösungsmittel

hydrochloric acid

1,2-dimethoxyethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter the metallation reaction
2. 2
   Sonstigethe volatile constituents were removed at 80° C. at a pressure of 10−2 bar
3. 3
   SonstigeThe residue obtained
4. 4
   Filtrationfiltered
5. 5
   Sonstigedried at 20° C.
6. 6
   SonstigeFor the further work-up, the product was recrystallized from a 3:1 mixture of water and methanol

Vorschrift

A solution of 3.07 g (16.5 mmol) of diphenylphosphine in 60 ml of 1,2-dimethoxyethane was admixed with 0.64 g (16.5 mmol) of potassium. After the metallation reaction was complete, 3.0 g (15.7 mmol) of sodium 2-(2-fluorophenyl)glycinate were added and the reaction mixture was heated at 80° C. for 3 hours. Subsequently, 10 ml of methanol were added and the volatile constituents were removed at 80° C. at a pressure of 10−2 bar. The residue obtained was suspended in 500 ml of dilute aqueous hydrochloric acid (pH=4) and filtered, and then dried at 20° C. and 10−2 bar. The yield was 4.7 g (89%). For the further work-up, the product was recrystallized from a 3:1 mixture of water and methanol. The 1H, 13C{1H} and 31P{1H} NMR spectra were recorded on a Bruker AC 250 spectrometer; the mass spectra were recorded on a Varian MAT 311 A instrument.

Quelle