HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-(2-Hydroxyethyl)piperazine → 2-[4-(2-hydroxyethyl)piperazin-1-yl]-N-[2,4-bis(methylthio)-6-methyl-3-pyridyl]acetamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-(2-Hydroxyethyl)piperazine | HCID 7677 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2-Bromo-N-(6-methyl-2,4-bis(methylthio)pyridin-3-yl)acetamide | HCID 22247149 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 2-[4-(2-hydroxyethyl)piperazin-1-yl]-N-[2,4-bis(methylthio)-6-methyl-3-pyridyl]acetamide | HCID 11689240 | 97% |
Reaction Steps
To a solution of 2-bromo-N-[2,4-bis(methylthio)-6-methyl-3-pyridyl]acetamide (6.41 g, 0.02 mol) in acetonitrile (120 ml) was added 1-(2-hydroxyethyl)piperazine(3.53 g, 0.027 mol), and then added potassium carbonate (3.75 g, 0.027 mol) with ice-cooling and the mixture was stirred at room temperature for 23 hours. The reaction solution was diluted with water and extracted with chloroform. The organic layer was washed with a saturated sodium chloride solution, dried over anhydrous sodium sulfate and concentrated in vacuo. The resulting residue was recrystallized from ethanol-ether to provide 7.19 g (yield 97%) of 2-[4-(2-hydroxyethyl)piperazin-1-yl]-N-[2,4-bis(methylthio)-6-methyl-3-pyridyl]acetamide as colorless needles.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06969711B2 |
| Source dataset | uspto-grants-2005_11 |
| ORD ID | ord-3fb4124b8cf14076bddb060391257354 |
| Source note | uspto-grants-2005_11 |