HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Amino-4-methylpyridine → HCID 18348765, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Amino-4-methylpyridine | HCID 1533 | — |
| Reactant | 4-Aminopyridine | HCID 1727 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Trichloromethanesulfenyl chloride | HCID 11666 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 18348765 | HCID 18348765 | 17% |
Reaction Steps
A solution of 3.2 g (30 mmol) of 2-amino-4-methylpyridine and 4.2 ml of triethylamine in 25 ml of dichloromethane is added dropwise at 0° C. to a solution of 3.3 ml (30 mmol) of trichloromethanesulphenyl chloride in 450 ml of dichloromethane, the mixture is stirred for 10 min and a solution of 2.8 g (30 mmol) of 4-aminopyridine and 12 ml of triethylamine in 100 ml of dichloromethane is added dropwise. After stirring at room temperature for 3 h, the mixture is poured into water and extracted with ethyl acetate, the extract is dried and concentrated, and the residue is chromatographed on silica gel (eluant ethyl acetate/isohexane 1:1). 1.2 g of title compound (17% of theory) of m.p. 144-145° C. are isolated.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06326378B1 |
| Source dataset | uspto-grants-2001_12 |
| ORD ID | ord-de4427a9f6a94383b01893d57c50e0de |
| Source note | uspto-grants-2001_12 |