HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 1-[2-(4-amino-1-piperidinyl)ethyl]-7-fluoro-2(1H)-quinoxalinone dihydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | tert-butyl{1-[2-(7-fluoro-2-oxoquinoxalin-1(2H)-yl)ethyl]piperidin-4-yl}carbamate | HCID 59397942 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 1-[2-(4-amino-1-piperidinyl)ethyl]-7-fluoro-2(1H)-quinoxalinone dihydrochloride | HCID 68817542 | 99% |
Reaction Steps
A solution of 1,1-dimethylethyl {1-[2-(7-fluoro-2-oxo-1(2H)-quinoxalinyl)ethyl]-4-piperidinyl}carbamate (8.72 g, 22.36 mmol) in methanol (90 ml) and dichloromethane (150 mL) was treated with 4 M hydrogen chloride in 1,4-dioxane (150 mL) (added in a slow stream, some exotherm and rapid precipitation observed) and stirred at room temperature for 2.5 h. The mixture was evaporated to dryness and the residue was triturated with ether. The solid was filtered off, washed with ether and dried to give the amine salt as a grey-green solid (8.06 g, 99%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08071592B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-c68060719ec646f6a90dbe073ba3f5a6 |
| Source note | uspto-grants-2011_12 |