HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 1-(3,4,5-Trimethoxyphenyl)piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | 3,4,5-Trimethoxyaniline | HCID 32285 | — |
| Reactant | Bis(2-chloroethyl)amine hydrochloride | HCID 522769 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Diglyme | HCID 8150 | — |
| Product | 1-(3,4,5-Trimethoxyphenyl)piperazine | HCID 3838765 | 14.5% |
Reaction Steps
11.9 g of 3,4,5-trimethoxyaniline, 11.6 g of bis(2-chloroethyl)amine hydrochloride, 9 g of anhydrous potassium carbonate, and 48 ml of diglyme were mixed and refluxed under heating for 28 hours. The reaction mixture was cooled, and was added into 100 ml of water. A concentrated aqueous potassium hydroxide solution was added to the aqueous mixture until the mixture had pH 12. The aqueous solution was then extracted with ethyl acetate. The ethyl acetate portion was washed with water, dried over anhydrous sodium sulfate, and placed under reduced pressure to distill offthe solvent. The residue was purified by silica gel column chromatography to give 2.37 g of the desired compound as a brown oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05446146 |
| Source dataset | uspto-grants-1995_08 |
| ORD ID | ord-40f3bf4533c941a18e7c8ddbb7e54bb4 |
| Source note | uspto-grants-1995_08 |