0-und m -P h e n y l e n b i s ( d i c h l o r p h o s p h a n 1 -,v i e l s e i t i g verwendbare S y n t h e s e b a u s t e i n e Von K u r t O r e w e l i e s und Hans P e t e r Latscha' Von den m o g l i c h e n P h e n y l e n b i s j d i h a l o g e n p h o s p h a n e n ) wurden b i s h e r n u r p -P h e n y l e n v e r b i n d u n g e n b e s c h r i e b e n Ill. Wir konnt e n nun 0-und m -P h e n y l e n U i s ( d i c h 1 o r p h o s p h a n ) 2 h e r s t e l l e n . D i e Synthesen(Schema 1) u b e r d i e e b e n f a l l s neuen Zwischenprod u k t e 0. 3 und 4 v e r l a u f e n i n a l l e n S c h r i t t e n i n g u t e n Ausb e u t e n . -4a ,a _ _ Schema 1 ~ a : o r t h o , a: meta --'Prof. O r . H.P. L a t s c h a , O i p l . Chem. K. O r e w e l i e s Anorganisch-Chemisches I n s t i t u t d e r U n i v e r s i t a t Im Neuenheimer F e l d 270, 0-6900 H e i d e l b e r g 1 -1416 -D i e R e a k t i o n von 0-o d e r m -B r o m p h e n y l d i c h l o r p h o s p h a n ( 2 . b ) m i t D i m e t h y l a m i n i n D i e t h y l e t h e r e r g i b t 0 -o d e r m-Bromphen y l b i s ( d i m e t h y l a m i n o j p h o s p h a n (3,a). f a r b l o s e F l u s s i g k e i t e n Z u r H e r s t e l l u n g von 0-o d e r m-Phenylenbis[bis(dimethylamino) p h o s p h a n l (4a.b) s e t z t man &,b m i t B u t y l l i t h i u m i n e t h e r is c h e r L o s u n g u r n und e r h a l t o r a n g e f a r b e n e , k l a r e Liisungen yon 0-o d e r m -L i t h i u m p h e n y l b i s ( d i m e t h y 1 a m i n o ) p h o s p h a n (3,:). Beim Z u t r o p f e n e t h e r i s c h e r LBsungen von E i s ( d i m et h y 1 a m i n o ) c h l o r p h o s p h a n b i l d e n s i c h 2.b. L i t h i u m c h l o r i d f a l l t a l s w e i B e r N i e d e r s c h l a g aus. % kann d e s t i l l i e r t , 2
der an der Oberflache von EPC-Vesikeln (74 A2171) sehr nahe; kristallines LPPC weist einen analogen helicalen Knick auf, der lediglich ein C-Atom naher am Kettenende IiegtC6'.Auch die fur LPPC-Kristalle charakteristische Doppelschichtstnrktur vom Typ ,,M//"161 findet sich in den Kristallen von 1 . NaSCN wieder, wobei Kopf-und Schwanzgruppen des Liganden jeweils zusammengelagert sind (Fig. 2). Interlamellare Kontakte uber die ,,anionischen" Seiten der Kronenetherringe hinweg (AuRenfltiche der Doppelschicht) bestehen nicht. Im Kristall von 1 . NaSCN hat die Doppelschicht einen Durchmesser von 2270 pm, in LPPC-Kristallen ist sie mit 2350 pmI6I nur geringfugig dicker.
The structure of the known compound O,O-Diphenyl-N-chlorophosphoramidate has been determined by X-ray diffraction. It consists of dimers, in which the monomers are connected by N-H···O hydrogen bonds. The O,O-Diethyl-N-chlorophosphoramidate homologue can be synthesized by various methods. At room temperature it is part of an equilibrium mixture with O,O-Diethyl-phosphoramidate and O,O-Diethyl-N,N-dichloro-phosphoramidate.
Abstract (C6H5O)2P(O)NHCl can be synthesized in 83-88% yield by direct hydrolysis of (C6H5O)2P(O)NCl2 in petroleumether solution. This first example of a new class of N-halogeno compounds, a colourless crystalline substance was characterized by 31P and 1H NMR, IR and mass spectroscopy as well as by elemental analysis.
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