HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → 1-(4-(3-(Aminomethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)-2-fluorophenyl)pyrrolidin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Tert-butyl (6-(3-fluoro-4-(2-oxopyrrolidin-1-yl)phenyl)-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methylcarbamate | HCID 57691433 | — |
| Product | 1-(4-(3-(Aminomethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)-2-fluorophenyl)pyrrolidin-2-one | HCID 57691283 | — |
Reaction Steps
A 50 mL recovery flask was charged with tert-butyl (6-(3-fluoro-4-(2-oxopyrrolidin-1-yl)phenyl)-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methylcarbamate (0.117 g, 0.274 mmol), TFA (0.0211 ml, 0.274 mmol), and DCM (0.0177 ml, 0.274 mmol), then stirred open to air at room temperature for 2 hours. The mixture was concentrated, then taken up in MeOH. K2CO3 was added, and this was stirred for 1 hour. The mixture was concentrated, then the residue was taken up in MeOH/CHCl3 then filtered. The filtrate was evaporated, taken up in water, then passed through a reverse phase C18 column, eluting with MeOH/DCM, then concentrated.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08524900B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-9cfd54ce9f1a403680f746923f72ea6e |
| Source note | uspto-grants-2013_09 |