Acetic Acid → HCID 71293376, compound

Participants

Reaction Conditions

Reaction Steps

150 mg (407 mmol) 1-methyl-1H-pyrrole-2-carboxylic acid[2-hydroxy-4-(4-methyl-6-oxo-5-propyl-1,4,5,6-tetrahydro-pyridazin-3-yl)-phenyl]-amide are placed in 5 mL dioxane. 300 μL (5.19 mmol) acetic acid and 140 mg (814 μmol) p-toluenesulphonic acid monohydrate are added and the mixture is stirred for 60 min in the microwave at 200° C. The reaction mixture is extracted successively with 10% sodium carbonate solution, 1% acetic acid, 10% sodium carbonate solution and saline solution. Then the solv. of the organic phase is eliminated i.V. and the residue is purified through silica gel. (Cyclohexane/EA) The solv. of the corresponding fractions is eliminated i.V. and the residue is crystallised with diethyl ether/petroleum ether.

Provenance & Evidence