Preparation of Some Hexaalkyl-phosphorous, Phosphoric and Phosphorothioic Triamides¹

Abstract

B.-To 10 ml. of refluxing aniline was carefully added 2.0 g. of 4-ammo-2-chloropyrido(3,2-d)pyrimidine (VII) and the heating was continued for 30 minutes. After cooling, the product was treated with 10 ml. of 50% ethanol containing a little sodium hydroxide, and filtered. The solid was recrystallized from ethanol to yield 0.6 g. of tan needles, m.p. 168-170°. A mixed melting point of this product with that of III prepared by method A was 168-170°.2,4-Bis-(dimethylamino)-pyrido(3,2-d)pyrimidme (II).-• This product was prepared from 2,4-dichloropyrido(3,2-d)-

Highly efficient copper-catalyzed N-arylation of alkylamines with aryl iodides using phosphoramidite as ligand

“…As shown in Scheme 1, the phosphoramidite ligands 2-7 were easily synthesized in high yields from the inexpensive, commercially available amines, PCl 3 and corresponding phenols by simple two steps [36][37][38]. Not only these ligands for solid were obtained by recrystallization rather than by using complex column chromatography but also they were stable for several weeks in air.…”

Metal catalysis in oxidation by peroxides. 24. Extraction of aqueous peroxomolybdenum species into organic media and their reactivity

“…An ethereal solution of PC13 (55 g, 0.4 mol) was dropwise added, over a 2-h period, to a solution of dibutyl amine (350g, 2.71 mol) in 500mL of anhydrous diethyl ether under vigorous stirring (10). After this time the mixture was allowed to return to room temperature and then refluxed for 6 h. The precipitated m i n e hydrochloride was filtered off, and carefully washed with ether.…”

A multinuclear NMR study of some cyclic phosphonic diamides

“…Substrates P[N(CH3h12OCH3 (A) and P[N(CH3h12CJIs (B) were synthesized by standard procedures [8,9]. Acetonitrile and CH 2 Cl 2 were dried over P20S and distilled, triethylamine was dried over KOH and distilled, benzene was distilled over Na, HN3 was synthesized in benzene by a standard procedure [10].…”