HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzoic acid, 4-fluoro-, ethyl ester → Ethyl 4-(3,4-dimethylpiperazin-1-yl)benzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzoic acid, 4-fluoro-, ethyl ester | HCID 67976 | — |
| Reactant | Dimethylpiperazine | HCID 198037 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | Ethyl 4-(3,4-dimethylpiperazin-1-yl)benzoate | HCID 57440404 | 36.2% |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
1,2-Dimethyl-piperazine (0.914 g, 8.00 mmol) and ethyl 4-fluorobenzoate (0.587 mL, 4 mmol) were dissolved in DMA (6 mL) and sealed into a microwave tube. The reaction was heated to 150° C. for 90 mins in the microwave reactor and cooled to room temperature. The reaction mixture was evaporated and the crude product was purified by silica column chromatography, eluting with 5% MeOH in DCM (containing 0.1% 0.880 ammonia). Pure fractions were evaporated to dryness to afford ethyl 4-(3,4-dimethylpiperazin-1-yl)benzoate (0.380 g, 36.2%) as a colourless waxy solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07737149B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-b9499f38f1d64c97b53dac0a329dbab8 |
| Source note | uspto-grants-2010_06 |