HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → N-Methylpyridine-4-methylamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | 4-(Chloromethyl)pyridinium chloride | HCID 74570 | — |
| Solvent | Water | HCID 962 | — |
| Product | N-Methylpyridine-4-methylamine | HCID 81436 | 66% |
Reaction Steps
To 4-picolyl chloride, hydrochloride (10 g, 0.06 mol) was added methylamine (50 mL of 40% aqueous solution, 0.58 mol), and the resulting purple solution was stirred at rt for 30 min, then poured into H2O. The mixture was extracted with CH2Cl2 (6×), and the combined organic extracts were evaporated. The residue was filtered under reduced pressure through a silica gel column, eluting with a solvent gradient of 0-10% MeOH/CHCl3 to provide the title compound as a light yellow oil (4.8 g, 66%): 1H NMR (CDCl3): d 8.50 (dd, 2H); 7.20 (dd, 2H); 3.70 (s, 2H); 2.40 (s, 3H); 1.70 (br, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06645989B2 |
| Source dataset | uspto-grants-2003_11 |
| ORD ID | ord-18d6f5c7d7a14a9eab5463f3054bc5ae |
| Source note | uspto-grants-2003_11 |