HuagongsheHuagongshe Chemistry Print Report · For research reference only
Morpholine → 2-Morpholinomethyl-4-chloropyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Morpholine | HCID 8083 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | 4-Chloro-2-methylpyridine | HCID 581392 | — |
| Catalyst | Benzoyl Peroxide | HCID 7187 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 2-Morpholinomethyl-4-chloropyridine | HCID 22025268 | — |
Reaction Steps
A mixture of the 2-methyl-4-chloropyridine (1.00 g, 7.84 mmol), NBS (1.42 g, 8.00 mmol) and benzoyl peroxide (˜10 mg) in 10 mL of CCl4 was heated at reflux for 5 h. After cooling down, the reaction mixture was filtered and filtrate was concentrated to give the crude products mixture, which was dissolved in DMF and treated with morpholine (1.00 mL) and K2CO3 (1 g). The mixture was stirred overnight. The mixture was then diluted with EtOAc, washed with water, brine, dried over Na2SO4, filtered and concentrated in vacuo. The crude product was purified by column chromatography on SiO2 to give 400 mg of the desired 2-morpholinomethyl-4-chloropyridine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07335657B2 |
| Source dataset | uspto-grants-2008_02 |
| ORD ID | ord-68121c0892204dfb9706e1ed8059c0bf |
| Source note | uspto-grants-2008_02 |