dichloro(ethoxy)phosphane

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Substantially the same procedure was followed as in Example 1, with 3.00 grams (34 mmol) N,N'-dimethylethylenediamine and 4.55 grams (31 mmol) ethylphosphorodichloridite to produce 2.31 grams of 1,3-dimethyl-2-ethoxy-1,3-diaza-2-phosphacyclopentane, ##STR25## as phosphorus amide catalyst.

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 68.7 g (0.5 mol) of phosphorustrichloride and 166 g (1 mol) of triethylphosphite, in which 2 grams of tris-2-ethylhexyl-phosphineoxide were dissolved, were simultaneously added dropwise into a flask within 30 minutes and mixed together by stirring while cooling at 48° to 52° C. At the end of the mixing process, the colorless slightly cloudy solution had the following composition: 6% C2H5OPCl2 ; 85% (C2H5O)2PCl; 5% (C2H5O)3P. In order to obtain pure phosphorous acid-diethyl ester-chloride, the high boiling constituents were first separated off at 10mm Hg and at a head temperature of 38° to 50° C. in a rapid distillation and the distillate was subsequently subjected to fine distillation. The product obtained at 33mm Hg and a head temperature of 60° to 62° C. was of 96% priority and its H-NMR agreed with the expected structure. were simultaneously added dropwise into a flask within 30 minutes mixed together while cooling at 48° to 52° C