Potassium Carbonate → HCID 18548249, compound

HRID 1265996Notes

Reaction equation

HRID 1265996 reaction equation
[CH3:1][C:2]1[NH:3][C:4](=[O:10])[CH2:5][C:6]=1[C:7]([NH2:9])=O.P(Cl)(Cl)(Cl)=O.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:1][C:2]1[NH:3][C:4](=[O:10])[CH2:5][C:6]=1[C:7]#[N:9]

Participants

5

Reactant 3

HCID 11430Potassium CarbonateHCID 24813Phosphorus oxychlorideHCID 185482534,5-Dihydro-2-methyl-5-oxo-1H-pyrrole-3-carboxamide

Product 1

HCID 18548249HCID 18548249, compound

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Procedure

A mixture of 0.9 g (4.6 mmol) of 2-methyl-5-oxo-4,5-dihydropyrrole-3-carboxamide, 1.4 g (9.2 mmol) of phosphorus oxychloride and 0.9 g (6.4 mmol) of potassium carbonate in 50 ml of acetone was refluxed for 6 h. The mixture was then concentrated and the resulting residue was chromatographed over silica gel (mobile phase: cyclohexane:ethyl acetate 10:1 to 1:1). This gave 0.15 g (19% of theory) of the desired product (IR: 2220 cm−1).

Workup

  1. temperaturewas refluxed for 6 h
  2. concentrationThe mixture was then concentrated
  3. customthe resulting residue was chromatographed over silica gel (mobile phase: cyclohexane:ethyl acetate 10:1 to 1:1)

Sources & evidence

ORD record
ord-433840dc73f74032bb157ec18fb6c4c0
Source dataset
uspto-grants-2003_04
Patent number
US06548451B1

Reaction notes

Loading…