HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Aminopyridine → HCID 86595791, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Aminopyridine | HCID 1727 | — |
| Reactant | HCID 22337024 | HCID 22337024 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Solvent | Dichloromethane methanol | HCID 21226129 | — |
| Product | HCID 86595791 | HCID 86595791 | — |
Reaction Steps
50 mg (0.1 mmol) of N-{2-[4-(bromomethyl)phenethyl]-1,3-dioxo-2,3-dihydro-1H-isoindol-4-yl}-5-chloro-2-thiophenecarboxamide are introduced a little at a time into a solution of 37.4 mg (0.4 mmol) of 4-aminopyridine in 4 ml 1,2-dichloroethane. The mixture is stirred at room temperature overnight and then diluted with dichloromethane/methanol (98:2), washed with sat. sodium bicarbonate solution, dried over magnesium sulfate and concentrated. The residue is crystallized using dichloromethane/ether and the solid is filtered off with suction and dried under high vacuum. Yield: 25.1 mg (37.2% of theory); MS (ESI): m/z (%)=517 (M+H, 100);); LC-MS (Method 7): rt (%)=3.42 (77).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06933295B2 |
| Source dataset | uspto-grants-2005_08 |
| ORD ID | ord-3b0c1f4b43994efb853f9371b108eac4 |
| Source note | uspto-grants-2005_08 |