Phosphorus trichloride → Diisopropylphosphoramidous dichloride

HRID 2120983Notes

Reaction equation

HRID 2120983 reaction equation
C(N([P:8]([N:10]([CH:14]([CH3:16])[CH3:15])[CH:11]([CH3:13])[CH3:12])[Cl:9])C(C)C)(C)C.P(Cl)(Cl)[Cl:18]>C(#N)C>[CH:11]([N:10]([P:8]([Cl:18])[Cl:9])[CH:14]([CH3:16])[CH3:15])([CH3:13])[CH3:12]

Participants

4

Reactant 2

HCID 24387Phosphorus trichlorideHCID 2733425Bis(diisopropylamino)chlorophosphine

Product 1

HCID 5139911Diisopropylphosphoramidous dichlorideYield 81%

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

Bis-(N,N-Diisopropylamino)chlorophosphine, 10 grams (37 mmols), was dissolved in 500 ml of anhydrous acetonitrile. Phosphorus trichloride, 5.16 grams (37 mmols), was added to the solution and the reaction was allowed to stir over-night at room temperature. The reaction was assayed for completion by 31P NMR of an aliquot of the reaction using an external lock. Complete conversion of the starting material at δ134 ppm to the product at δ165 ppm was observed. The solvent was evaporated from the reaction mixture on a rotary evaporator and the resulting oil distilled under vacuum yielding 5.7 grams of product (81% yield).

Workup

  1. customThe solvent was evaporated from the reaction mixture on a rotary evaporator
  2. distillationthe resulting oil distilled under vacuum

Sources & evidence

ORD record
ord-04fe239c28b44c1ea759cbe533d50c4d
Source dataset
uspto-grants-2004_02
Patent number
US06693187B1

Reaction notes

Loading…