HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86659261, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | HCID 86659260 | HCID 86659260 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86659261 | HCID 86659261 | — |
Reaction Steps
ethyl 4-{[2-(tert-butoxycarbonyl)-5-(4-methylpiperazin-1-yl)phenyl](trifluoroacetyl)amino}piperidine-1-carboxylate (2.15 g, 3.960 mmol) was dissolved in dry dichloromethane (8 mL) under nitrogen atmosphere. A 4 M solution of HCl in dioxane (9.9 mL, 39.6 mmol, 10 eq) was then added dropwise and the mixture was stirred at room temperature. After 5 hours 5 more equivalents of HCl were added and the reaction was stirred at room temperature overnight. The mixture was evaporated to dryness and stripped twice with DCM. It was then taken up with DCM/dioxane 1:3 and slurried for 1 hour. The solid was filtered, washed with ether and dried under vacuum at 50° C. for 1 hour. 1.78 g of title compound were obtained as a beige powder (86% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08354399B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-f0e4478fb30b4824b613905ebd0d5eb1 |
| Source note | uspto-grants-2013_01 |