Reaktion #310494

Reaktionsgleichung

ethyl N-trifluoroacetyl-N-(dichlorophosphonomethyl)glycinate

pentafluorophenylhydrazine

→

ethyl N-trifluoroacetyl-N-(bis(pentafluorophenylhydrazino)phosphonomethyl)glycinate

Lösungsmittel

tetrahydrofuran

tetrahydrofuran

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationfiltered
2. 2
   WaschenThe filtrate was washed with water
3. 3
   Sonstigedried
4. 4
   Einengenconcentrated in vacuo
5. 5
   Sonstigeto yield a dark red-brown solid
6. 6
   WaschenThis solid was washed several times with 70% ether in petroleum ether

Vorschrift

To a solution of pentafluorophenylhydrazine (3.96 g, 0.02 mole) in 40 ml. of tetrahydrofuran at 0° C. was added over 1/2 hour ethyl N-trifluoroacetyl-N-(dichlorophosphonomethyl)glycinate (1.65 g, 0.005 mole) in 40 ml. of tetrahydrofuran. The reaction mixture was allowed to warm to room temperature and stir for 2 hours, then filtered. The filtrate was washed with water, dried, and concentrated in vacuo to yield a dark red-brown solid. This solid was washed several times with 70% ether in petroleum ether to yield ethyl N-trifluoroacetyl-N-(bis(pentafluorophenylhydrazino)phosphonomethyl)glycinate, m.p. 100°-110° C.

Quelle