Phosphoroxy chloride

Amino4-chlorodiphenylamine-2 -carboxylic(4 -methyl)piperazide Phosphoroxy chloride... 

A mixture of 6 parts DL-2-(acetylimno)-3-[2-hydroxy-2-(2-thienyl)ethyl]thiazoline and 80 parts phosphoroxy-chloride is heated in a water-bath for 2 hours at a temperature of 100°C. On cooling, the reaction mixture is poured into water. The whole is alkalized with ammonium hydroxide solution and extracted with toluene. The extract is dried over magnesium sulfate and evaporated in vacuum. The oily residue is dissolved in 40 parts boiling 2-propanol. To this warm solution is added a warm solution of an equivalent quantity of oxalic acid dihydrate in 2-propanol. After cooling to room temperature, the precipitated salt is filtered off and dried in vacuum, yielding DL-5,6-dihydro-6-(2-thienyl)imidazo[2,l-b]thiazole oxalate MP 193°-194°C. 

Chlor-ethyl)- -2-oxid E2, 384 2-Chlormethyl- -2-oxid XII/1, 496 2-Chlor-2-(4-methyl-phenylsulfonylimino)- E2, 809 2-Chlor- -2-oxid Xll/2, 280 E2, 503, 897 aus l,2-Bis-[2-oxo-benzo-l,3,2-dioxaphos-phol-2-yloxy]-benzol und Phosphoroxy-chlorid XII/2, 283... 

Several alternative procedures have been developed for chemical synthesis of 41. Acetals of the dimer of 47 can be phosphoryated using phosphoroxy chloride [184] or diphenyl chlorophosphate [185], or by phosphitylation then oxidation [186]. After phosphate deprotection, free 41 is obtained, by acid hydrolysis, in overall yields of up to 60%. New procedures have recently been developed by controlled successive substitutions of dibromoacetone [187, 188] or by controlled hydrolysis of a cyclic phosphate diester of 47 [189]. 

---