HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen Bromide → 1-Tert-butylpiperazine dihydrobromide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 12268380 | HCID 12268380 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 1-Tert-butylpiperazine dihydrobromide | HCID 21906354 | — |
Reaction Steps
To crude 3-[2-(tert-butylamino)ethyl]oxazolidin-2-one (1.18 g, 6.33 mmol) was added acetic acid (8.8 mL) and then 45% hydrobromic acid in acetic acid (19.5 mL). The reaction solution was stirred at room temperature for 3 d, poured into dichloromethane (250 mL), and filtered to give 1.87 g of a brown solid. The solid was heated at reflux in n-butanol for 2 d and the reaction mixture concentrated in vacuo. The residual solid was slurried in 3:1 diethyl ether:dichloromethane and filtered. The filtered solid was heated in ethanol, cooled to room temperature, and filtered to give 0.57 g (30%) of a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06635657B1 |
| Source dataset | uspto-grants-2003_10 |
| ORD ID | ord-886c57bbc59c4a4eb83c88f7ebbf207f |
| Source note | uspto-grants-2003_10 |