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ChemicalBook CAS DataBase List DIETHYL CHLOROPHOSPHITE
589-57-1

DIETHYL CHLOROPHOSPHITE synthesis

13synthesis methods
-

Yield:589-57-1 82% ，122-52-1 18%

Reaction Conditions:

with triethylamine in toluene

Steps:

15 Example 15
Synthesis of phosphorochloridite 1e and phosphorodichloridite 2e. This example shows that aliphatic phosphorochloridites and phosphorodichloridites can be produced in good selectivity. [0044] A temperature controlled 300 ml baffled round bottom flask was charged with a solution of 25 ml 2.0 molar PCl3 in toluene. Under vigorous stirring a solution of 25 ml 2.0 molar triethylamine in toluene and a solution of 25 ml 2.0 molar ethylalcohol in toluene were added separately and concurrently via a dual syringe pump over a period of 100 min. During the addition period the reaction temperature was maintained at -10° C. The 31P NMR analysis exhibited transformation to the corresponding dichloridite 2e in 94% selectivity. Another 25 ml of each 2.0 molar triethylamine solution in toluene and 2.0 molar ethylalcohol solution in toluene were added separately and concurrently via dual syringe pump over a period of 100 min. The 31P NMR analysis exhibited transformation to the corresponding chloridite 1e in 70% overall selectivity. Another 4.7 ml of each 2.0 molar triethylamine solution in toluene and 2.0 molar ethylalcohol solution in toluene were added separately and concurrently via a dual syringe pump. The final product distribution was 82% phosphorochloridite 1e and 18% triethylphosphite. No Ethylchloride was formed.

References:

Ritter, Joachim C. US2004/106815, 2004, A1 Location in patent:Page 5-6

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