Phosphorus oxychloride → HCID 20494275, compound

HRID 1075144Notes

Reaction equation

HRID 1075144 reaction equation
O[CH2:2][CH2:3][N:4]1[CH:9]=[C:8]([Cl:10])[CH:7]=[N:6][C:5]1=[O:11].P(Cl)(Cl)([Cl:14])=O>>[Cl:14][CH2:2][CH2:3][N:4]1[CH:9]=[C:8]([Cl:10])[CH:7]=[N:6][C:5]1=[O:11]

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 20494293HCID 20494293, compound

Product 1

HCID 20494275HCID 20494275, compoundYield 52%

Procedure

1-(2-Hydroxyethyl)-5-chloropyrimid-2-one (0.001 mol) and phosphorus oxychloride (5 ml) were heated together at 80° C. for 60 min. before the solution was evaporated at reduced pressure. The residue was triturated with chloroform before dissolution in water (4 ml) and neutralisation with sodium bicarbonate. Chloroform extraction and evaporation left a solid which was recrystallised from ethyl acetate, yield 52%, m.p. 167°-168° C. (Found: C, 37.20; H, 3.20; Calc for C6H6Cl2N2O: C, 37.34; H 3.13).

Workup

  1. customwas evaporated at reduced pressure
  2. customThe residue was triturated with chloroform before dissolution in water (4 ml)
  3. extractionChloroform extraction and evaporation
  4. waitleft a solid which
  5. customwas recrystallised from ethyl acetate, yield 52%, m.p. 167°-168° C. (Found: C, 37.20; H, 3.20; Calc for C6H6Cl2N2O: C, 37.34; H 3.13)

Sources & evidence

ORD record
ord-8db86e3397644d33bbaeca438729fc9e
Source dataset
uspto-grants-1983_07
Patent number
US04395406

Reaction notes

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