HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Chloropyridine → HCID 10797035, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Chloropyridine | HCID 12288 | — |
| Reactant | 1-Aminopyrrole | HCID 136589 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Diglyme | HCID 8150 | — |
| Solvent | Sodium Carbonate | HCID 10340 | — |
| Product | HCID 10797035 | HCID 10797035 | 57.1% |
Reaction Steps
A solution of 4-chloropyridine (15 g) and N-aminopyrrole (18 g) in 225 ml of diglyme was stirred at 150° C. for one hour and thereafter cooled, diluted with water and basified with sodium carbonate. The mixture was extracted with ethyl acetate, and the organic extract was dried over anhydrous magnesium sulfate, filtered and evaporated to an oil. This oil was purified by high performance liquid chromatography (HPLC hereafter) using silica gel and ethyl acetate to give 12 g of a solid, mp 150° C. Five grams of the solid was recrystallized twice from benzene to give 2.8 g of crystals, mp 153°-154° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05039687 |
| Source dataset | uspto-grants-1991_08 |
| ORD ID | ord-507cf55a59ba4439b62427a4b46d8437 |
| Source note | uspto-grants-1991_08 |