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 | Chloroform | HCID 6212 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 18348765 | HCID 18348765 | 17% |
Reaction Steps
To a solution of 3.3 ml (30 mmol) trichloromethanesulphenic acid chloride in 450 ml dichloromethane one adds dropwise at 0° C. a solution of 3.2 g (30 mmol) 2-amino-4-methylpyridine and 4.2 ml triethylamine in 25 ml. dichloromethane, stirs for 10 min and adds dropwise thereto a solution of 2.8 g (30 mmol) 4-aminopyridine and 12 ml triethylamine in 100 ml dichloromethane. After 3 h stirring at room temperature, one pours into water, extracts with ethyl acetate, dries the extract, evaporates and chromatographs on silica gel (elution agent ethyl acetate/isohexane 1:1), One isolates 1,2 g of title compound (17% of theory) of the m.p. 144°-145° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05447934 |
| Source dataset | uspto-grants-1995_09 |
| ORD ID | ord-861fec16abd843c887497a0fbf115067 |
| Source note | uspto-grants-1995_09 |