Diethyl chlorophosphate → HCID 573023, compound

HRID 1703434Notes

Reaction equation

HRID 1703434 reaction equation
[CH2:1]([O:3][P:4](Cl)(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2].[N-:10]=[N+:11]=[N-:12].[Na+]>C(#N)C>[P:4]([N:10]=[N+:11]=[N-:12])([O:5][CH2:6][CH3:7])([O:3][CH2:1][CH3:2])=[O:8]

Participants

4

Reactant 2

HCID 13139Diethyl chlorophosphateHCID 33557Sodium Azide

Product 1

HCID 573023HCID 573023, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

Following the procedure of Shioiri, Nimomiya, and Yamada, J. Amer. Chem. Soc., 94, 6203 (1972), 5.13 g (0.03 mole) of diethylphosphorochloridate and 1.95 g (0.03 mole) of sodium azide were added to 50 ml dry acetonitrile purified by distillation from calcium hydride under a nitrogen atmosphere. The slurry was stirred at reflux for 1 hour, cooled and filtered by gravity to remove the solid precipitate. The acetonitrile solvent was distilled under vacuum. The sample was isolated by vacuum distillation.

Workup

  1. distillationpurified by distillation from calcium hydride under a nitrogen atmosphere
  2. temperatureat reflux for 1 hour
  3. temperaturecooled
  4. filtrationfiltered by gravity
  5. customto remove the solid precipitate
  6. distillationThe acetonitrile solvent was distilled under vacuum
  7. customThe sample was isolated by vacuum distillation

Sources & evidence

ORD record
ord-e5db7492b9b145b3b4ad572424dd786b
Source dataset
uspto-grants-1978_11
Patent number
US04124356

Reaction notes

Loading…