HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 4-(4-Benzyl-piperazin-1-YL)-benzoic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Methyl 4-fluorobenzoate | HCID 67878 | — |
| Reactant | 1-Benzylpiperazine | HCID 75994 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 4-(4-Benzyl-piperazin-1-YL)-benzoic acid methyl ester | HCID 53406803 | — |
Reaction Steps
4-Fluorobenzoic acid methyl ester (200 mmol), 1-benzyl-piperazine (300 mmol), and potassium carbonate (300 mmol) are suspended in acetonitrile (400 ml) and stirred under reflux for 6 days. After evaporation of the solvent, the residue is dissolved in water and extracted three times with diethylether. The extract is dried over sodium sulfate and evaporated. The residue is purified by flash chromatographic on silica gel with (CH2Cl2 first, then CH2Cl2/MeOH=15:1) as mobile phase. The product containing fractions are combined and evaporated. The residue is suspended in diethylether/pentane and the solid filtered of and dried (vacuum). A powder with mp. 105-107° C. is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06642239B2 |
| Source dataset | uspto-grants-2003_11 |
| ORD ID | ord-643943c8625e4bde87b0e059975f3e40 |
| Source note | uspto-grants-2003_11 |