Phosphorus pentachloride → HCID 20077492, compound

HRID 2379701Notes

Reaction equation

HRID 2379701 reaction equation
O[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][C:10]=2[CH3:12])[N:5]=[N:4][C:3]=1[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.P(Cl)(Cl)(Cl)(Cl)[Cl:20]>O=P(Cl)(Cl)Cl>[Cl:20][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][C:10]=2[CH3:12])[N:5]=[N:4][C:3]=1[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

Participants

4

Reactant 2

HCID 24819Phosphorus pentachlorideHCID 178424058HCID 178424058, compound

Product 1

HCID 20077492HCID 20077492, compound

Reagents, catalysts & solvents 1

HCID 24813Phosphorus oxychlorideSolvent

Procedure

27.3 g (0.116 mol) of the compound from Example VI are boiled under reflux with 18.3 g of PCl5 and 200 ml of POCl3 for 18 h. The mixture is added to ice with good stirring and extracted with methylene chloride, and the organic phase is washed with saturated NaHCO3 solution, dried and evaporated in vacuo. 12 g (41% crude yield) of a solid are obtained, which after chromatography has a m.p. of 128° C.

Workup

  1. additionThe mixture is added to ice
  2. extractionextracted with methylene chloride
  3. washthe organic phase is washed with saturated NaHCO3 solution
  4. customdried
  5. customevaporated in vacuo
  6. custom12 g (41% crude yield) of a solid are obtained

Sources & evidence

ORD record
ord-9875e2594d414900a5527594c3b73cc7
Source dataset
uspto-grants-1994_11
Patent number
US05364855

Reaction notes

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