HCID 824395, compound → HCID 19349977, compound

HRID 1045381Notes

Reaction equation

HRID 1045381 reaction equation
[C:1]([NH:4][NH:5][C:6](=[O:14])[C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([I:13])[CH:8]=1)(=O)[CH3:2]>O=P(Cl)(Cl)Cl>[I:13][C:9]1[CH:8]=[C:7]([C:6]2[O:14][C:1]([CH3:2])=[N:4][N:5]=2)[CH:12]=[CH:11][CH:10]=1

Participants

3

Reactant 1

HCID 824395HCID 824395, compound

Product 1

HCID 19349977HCID 19349977, compound

Reagents, catalysts & solvents 1

HCID 24813Phosphorus oxychlorideSolvent

Procedure

The product obtained in Step A above (2.9 g, 9.54 mmol) is heated at 120° C. for 3 hours in 35 ml of POCl3. After evaporation of POCl3, the residue is taken up in toluene and the mixture is evaporated to dryness again. The residue from evaporation is dissolved in ethyl acetate and the organic phase is washed with, in succession, 10% NaHCO3 solution, water and then brine. The organic phase is dried over MgSO4 to yield, after evaporation, the expected product in the form of a creamy white solid.

Workup

  1. customAfter evaporation of POCl3
  2. customthe mixture is evaporated to dryness again
  3. customThe residue from evaporation
  4. dissolutionis dissolved in ethyl acetate
  5. washthe organic phase is washed with, in succession, 10% NaHCO3 solution, water
  6. dry with materialThe organic phase is dried over MgSO4
  7. customto yield
  8. customafter evaporation

Sources & evidence

ORD record
ord-04d462ce02bc451a82f8f65efa7e4724
Source dataset
uspto-grants-2013_10
Patent number
US08569285B2

Reaction notes

Loading…