HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl isocyanate → HCID 68840036, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl isocyanate | HCID 8022 | — |
| Reactant | Sodium bis(trimethylsilyl)amide | HCID 2724254 | — |
| Reactant | HCID 68836465 | HCID 68836465 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68840036 | HCID 68840036 | — |
Reaction Steps
A mixture of 5-(3-dimethylamino-pyrrolidin-1-yl)-7-pyridin-3-yl-[1,2,4]triazolo[1,5-a]pyridin-2-ylamine (0.190 g, 0.6 mmol), and NaHMDS (1.4 ml of 1 M solution in THF, 1.4 mmol) in anhydrous THF (100 ml) was stirred at room temperature for 45 minutes. EtNCO (0.5 ml, 6.3 mmol) was added and the resulting reaction mixture was stirred at room temperature overnight. The reaction was quenched with HCl (0.35 ml of 4 M solution in dioxane). Solvent was evaporated and the resultant material was purified by column chromatography on silica gel (1% NEt3, 0-10% MeOH in CH2Cl2 as eluant), followed by trituration in EtOH, to afford the desired compound as a solid. Mp. 248-250° C. MS (APCI+) 395 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07524860B2 |
| Source dataset | uspto-grants-2009_04 |
| ORD ID | ord-a89029beee654409803a8840fa130a98 |
| Source note | uspto-grants-2009_04 |