Phosphorus oxychloride → HCID 21438899, compound

HRID 329167Notes

Reaction equation

HRID 329167 reaction equation
[CH2:1]([N:3]1[C:8](=[O:9])[CH:7]([CH2:10][CH3:11])[C:6](=O)[NH:5][C:4]1=[S:13])[CH3:2].P(Cl)(Cl)([Cl:16])=O>O>[CH2:1]([N:3]1[C:8](=[O:9])[C:7]([CH2:10][CH3:11])=[C:6]([Cl:16])[NH:5][C:4]1=[S:13])[CH3:2]

Participants

4

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 14795121HCID 14795121, compound

Product 1

HCID 21438899HCID 21438899, compoundYield 70%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

10 G. OF 3,5-DIETHYL-2-THIOBARBITURIC ACID IS CHLORINATED, AFTER THE ADDITION OF A FEW DROPS OF WATER, WITH EXCESS PHOSPHORUS OXYCHLORIDE (APPROXIMATELY 100 ML.) UNDER HEATING FOR 3/4 HOUR. The excess phosphorus oxychloride is distilled off, and the residue is poured on ice. The desired reaction product is crystallized during this step and melts, after recrystallization from aqueous ethanol, completely at 228° C. Yield: 70%

Workup

  1. temperature) UNDER HEATING FOR 3/4 HOUR
  2. distillationThe excess phosphorus oxychloride is distilled off
  3. additionthe residue is poured on ice
  4. customThe desired reaction product
  5. customis crystallized during this step and melts
  6. customafter recrystallization from aqueous ethanol
  7. customcompletely at 228° C

Sources & evidence

ORD record
ord-f42f5ea4e36b4379bfe97e7f4a32e7fb
Source dataset
uspto-grants-1977_04
Patent number
US04020070

Reaction notes

Loading…