Phosphorus trichloride → Phosphorus trichloride

HRID 477756Notes

Reaction equation

HRID 477756 reaction equation
C1C=CC([P:7]([Cl:10])([Cl:9])=[O:8])=CC=1.[P:11]([Cl:14])([Cl:13])[Cl:12]>>[P:11]([Cl:14])([Cl:13])[Cl:12].[P:7]([Cl:10])([Cl:12])([Cl:9])=[O:8]

Participants

4

Reactant 2

HCID 24387Phosphorus trichlorideHCID 69990Phenylphosphonic dichloride

Product 2

HCID 24387Phosphorus trichlorideHCID 24813Phosphorus oxychloride

Conditions

Temperature
600 °C

Procedure

100 g (=0.513 mol) of phenylphosphonyl dichloride and 200 g (=1.45 mol) of phosphorus trichloride were mixed. This mixture was introduced dropwise, over the course of 3 hours, into a vertical quartz tube which was 60 cm long, filled with 6 mm diameter quartz Raschig rings, was flushed with nitrogen and was located in an electric oven heated to 600° C. The reaction mixture collecting in the trap was again introduced dropwise, over the course of 2 hours, into the quartz tube at 600° C. The reaction mixture now produced was distilled in vacuo. Apart from unreacted phosphorus trichloride and phosphorus oxychloride, 80 g of a distillate were obtained which, on the basis of a 31P NMR spectrum, had the following composition:

Workup

  1. additionThis mixture was introduced dropwise, over the course of 3 hours, into a vertical quartz tube which
  2. customwas flushed with nitrogen
  3. customwas located in an electric oven
  4. customThe reaction mixture collecting in the trap
  5. additionwas again introduced dropwise, over the course of 2 hours, into the quartz tube at 600° C
  6. customThe reaction mixture now produced
  7. distillationwas distilled in vacuo

Sources & evidence

ORD record
ord-0e108b39327747698e0b2ec79fb4d035
Source dataset
uspto-grants-1989_12
Patent number
US04889661

Reaction notes

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