Process for the production of S-alkyl phosphoro dihalogenidodith

Details Process for the production of S-alkyl phosphoro dihalogenidodith Process for the production of S-alkyl phosphoro dihalogenidodith

1975-10-23

1977-07-12

Raymond, Richard L.

Chemistry of carbon compounds

Dipeptides, e.g., aspartame, anserine, carnosine, etc.

260948, 260950, 260958, 260960, 260985, C07F 920

Patent

active

040354490

ABSTRACT:
S-alkyl phosphoro dihalogenidodithioate is prepared by the reaction of alkyl mercaptan with a phosphorous trihalogenide (PX.sub.3) and elemental sulfur in the presence of a sulfurization catalyst. The alkyl mercaptan may be reacted with the phosphorous trihalogenide either in a separate vessel or in the same vessel as the subsequent sulfurization of these reaction products. Sufficient sulfur is used to sulfurize substantially all phosphorous atoms present to a penta-valent state. If a sufficient excess of phosphorous trihalogenide is not used in the initial reaction either additional phosphoroustrihalogenide or PSX.sub.3 is added so that at the end of sulfurization there is at least about one mole of PSX.sub.3 present for each mole of S,S-dialkyl phosphorohalogenido trithioate and two moles for each mole of S,S,S-trialkyl phosphorotetrathioate present. The PSX.sub.3 and dialkyl and trialkyl compounds are held at sufficient temperature for a sufficient time to convert them substantially to S-alkyl phosphorodihalogenidodithioate. A period of at least about 1 hour at not less than about 150.degree. C is preferred. The PSX.sub.3 and product (S-alkyl phosphorodihalogenidodithioate) may be removed as distillation overheads and the residue left as a heel for subsequent cycles.

REFERENCES:
patent: 2943107 (1960-06-01), Rattenbury et al.
patent: 3457306 (1969-07-01), Baker et al.
patent: 3879500 (1975-04-01), Uhing et al.
Houben-Weyl, Methoden der Organischen Chemie, 12/2, (1964), pp. 682, 683, 739 and 740.

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