Antimony pentachloride → HCID 86738015, compound

HRID 1578157Notes

Reaction equation

HRID 1578157 reaction equation
[Sb:1]([Cl:6])([Cl:5])([Cl:4])([Cl:3])[Cl:2].[CH2:7]([O:11][P:12]([O:19]CCCC)([O:14]CCCC)=[O:13])[CH2:8][CH2:9][CH3:10]>C(Cl)Cl>[Sb:1]([Cl:6])([Cl:5])([Cl:4])([Cl:3])[Cl:2].[P:12]([O-:19])([O-:14])([O:11][CH2:7][CH2:8][CH2:9][CH3:10])=[O:13]

Participants

4

Reactant 2

HCID 24294Antimony pentachlorideHCID 31357Tributyl Phosphate

Product 1

HCID 86738015HCID 86738015, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent3×

Procedure

In a round bottom flask under a nitrogen atmosphere, 8.01 g (0.0268 M) of antimony pentachloride was dissolved in 100 ml of methylene chloride. To this yellow solution was added dropwise with stirring a solution of 7.13 g (0.0268 M) of tributylphosphate in 20 ml of methylene chloride. The addition was accomplished at a rate such that the exotherm did not become excessive, the temperature being kept below the reflux temperature of methylene chloride (cooling should not be required). By the end of the addition, the initial yellow color had changed to a light brown. The reaction mixture was stirred at ambient temperature for one hour, after which time the solvent was removed by evaporation at reduced pressure. The dark brown liquid was thoroughly dried in vacuo (0.1 mm Hg). NMR (CDCl3, TMS) δ4.45(9H,q,J=6.0 Hz), 1.85(6H,m), 1.50(6H,m), 1.00(6H,t,J=6.7 Hz).

Workup

  1. additionTo this yellow solution was added dropwise
  2. additionThe addition
  3. temperaturecooling should not
  4. additionBy the end of the addition
  5. customafter which time the solvent was removed by evaporation at reduced pressure
  6. customThe dark brown liquid was thoroughly dried in vacuo (0.1 mm Hg)

Sources & evidence

ORD record
ord-8d1e7f37fff144e99c684223afe8a55a
Source dataset
uspto-grants-1981_09
Patent number
US04291145

Reaction notes

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