HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → 4-((4-Methylpiperazin-1-yl)methyl)-3-(trifluoromethyl)benzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Ethyl 4-((4-methylpiperazin-1-yl)methyl)-3-(trifluoromethyl)benzoate | HCID 23145917 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 4-((4-Methylpiperazin-1-yl)methyl)-3-(trifluoromethyl)benzoic acid | HCID 23145880 | — |
Reaction Steps
To a solution of ethyl 4-(4-methyl-piperazin-1-ylmethyl)-3-trifluoromethyl-benzoate (7.23 g, 21.1 mmol, 1.0 eq.) in ethanol (40 ml) is added 1M NaOH (30.6 ml, 30.6 mmol, 1.4 eq.). After stirring for 2 h at room temperature a clear pale yellow solution is obtained. The mixture is evaporated to a volume of 30 ml. Then, the solution is adjusted to pH 7 by addition of 1M HCl and the solvent is stripped off. The residue is taken up three times in toluene (70 ml) and evaporated. The crude material is dissolved in ethanol/THF 1:9 (150 ml), filtered, evaporated, triturated with ethyl acetate, and vacuum dried at 60° C. over night to afford a beige powder: HPLC: tR=3.61 min (purity: >99%, gradient A), ESI-MS: 303.3 [MH]+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08552002B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-54b6d96ada1d41bfbd5ab64c41de56bb |
| Source note | uspto-grants-2013_10 |