Phosphorus trichloride → HCID 131711284, compound

HRID 1111627Notes

Reaction equation

HRID 1111627 reaction equation
P(Cl)(Cl)[Cl:2].[CH2:5]([O:7][P:8]([O:12]CC)[O:9][CH2:10][CH3:11])[CH3:6].C(OP(Cl)Cl)C.P(Cl)(OCC)OCC>>[Cl-:2].[CH2:5]([O:7][P:8]([OH:12])[O:9][CH2:10][CH3:11])[CH3:6]

Participants

5

Reactant 4

HCID 24387Phosphorus trichlorideHCID 31215Triethyl phosphite2×HCID 68530Ethyl phosphorochloriditeHCID 73905Ethyl dichlorophosphite

Product 1

HCID 131711284HCID 131711284, compound

Procedure

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.

Workup

  1. additionwere simultaneously added dropwise into a flask within 30 minutes
  2. additionmixed together
  3. temperaturewhile cooling at 48° to 52° C

Sources & evidence

ORD record
ord-510541e6a61049298adb2bbaa63a03bc
Source dataset
uspto-grants-1978_10
Patent number
US04118435

Reaction notes

Loading…