HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → Triethylamine hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | 1-(2-Hydroxyethyl)piperazine | HCID 7677 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Triethylamine hydrochloride | HCID 11130 | — |
| Product | 1-Acetyl-4-(2-hydroxyethyl)piperazine | HCID 4739629 | — |
Reaction Steps
2-Piperazinoethanol (7.81 g, 60 mmoles) and triethylamine (8.36 ml, 66 mmoles) were dissolved in 100 ml of methylene chloride and cooled to 0°-5° C. Acetyl chloride (4.28 ml, 60 mmoles) in 20 ml of methylene chloride was added and the reaction mixture warmed to room temperature, held for 2 hours, and then evaporated in vacuo to dry solids. The solids were triturated with four portions of warm ether. The triturates were combined, dried over anhydrous magnesium sulfate, filtered and evaporated to yield 2-(4-acetylpiperazino)ethanol as an oil [7.5 g; free of triethylamine and triethylamine hydrochloride by pnmr assay; Rf 0.3 (methanol/10% acetic acid)].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04427679 |
| Source dataset | uspto-grants-1984_01 |
| ORD ID | ord-643b4633e9bc40999157160e5d9fc3ae |
| Source note | uspto-grants-1984_01 |