HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 22632924, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 22633001 | HCID 22633001 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 22632924 | HCID 22632924 | 88.1% |
Reaction Steps
A solution of ethyl 2-cyclopropylamino-5-fluoro-6-pyrrolidinyl-3-pyridine-carboxylate (Example E-2, 270 mg, 0.92 mmol) and NaOH (360 mg, 9.0 mmol) in water (1 mL), THF (2 mL), and MeOH (1 mL) was refluxed for 3 hours. The mixture was cooled to room temperature, acidified with dilute HCl to pH 6, and evaporated under reduced pressure. The residue was mixed with 10% MeOH/dichloromethane (40 mL), dried on sodium sulfate, filtered, and evaporated. The solid residue was further washed with hexane and dried in vacuo, giving 215 mg of the title compound as powder, mp 64-66° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06331538B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-90b373742dbc43b6a51852d2bc6e5833 |
| Source note | uspto-grants-2001_12 |