HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 4-chloro-2-(N-(2-morpholin-4-ylethyl)carbamoyl)pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 2-Morpholinoethylamine | HCID 408285 | — |
| Reactant | Methyl 4-chloropyridine-2-carboxylate--hydrogen chloride (1/1) | HCID 16655470 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4-chloro-2-(N-(2-morpholin-4-ylethyl)carbamoyl)pyridine | HCID 23614579 | 95.4% |
Reaction Steps
To a solution of methyl 4-chloropyridine-2-carboxylate HCl salt (Method A2, Step 2; 1.01 g, 4.86 mmol) in THF (20 mL) was added 4-(2-aminoethyl)morpholine (2.55 mL, 19.4 mmol) dropwise and the resulting solution was heated at the reflux temp. for 20 h, cooled to room temp., and treated with water (50 mL). The resulting mixture was extracted with EtOAc (50 mL). The organic layer was dried (MgSO4) and concentrated under reduced pressure to afford 4-chloro-2-(N-(2-morpholin-4-ylethyl)carbamoyl)pyridine as a yellow oil (1.25 g, 95%): TLC (10% MeOH/90% EtOAc) Rf 0.50.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08841330B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-ca6a6a4905ed4e3996dd133866f1f1e6 |
| Source note | uspto-grants-2014_09 |