HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 69920753, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethylamine | HCID 8021 | — |
| Reactant | Trimethylaluminum | HCID 16682925 | — |
| Reactant | HCID 23552715 | HCID 23552715 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 69920753 | HCID 69920753 | — |
Reaction Steps
To a solution of 35 mg (0.44 mmol) diethylamine in 0.5 ml dioxane was added 0.5 ml methylaluminoxane (10% in toluene) (in a variant trimethylaluminium was used instead of methylaluminoxane which proofed to give comparable results) and stirred for 1 h at room temperature. 31 mg (0.11 mmol) 5-Amino-2-(5-methyl-furan-2-yl)-[1,2,4]triazolo[1,5-a]pyridine-7-carboxylic acid methyl ester in 1 ml dioxane was added and the mixture was heated to 80° C. for 72 h. After addition of 0.4 ml 1N HCl the mixture was evaporated to dryness and the residue was taken up in 1.5 ml DMSO, filtered, and the title compound was isolated by reversed phase HPLC eluting with a water/acetonitrile gradient to yield 8.6 mg (25%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06506772B1 |
| Source dataset | uspto-grants-2003_01 |
| ORD ID | ord-b211d80b113745f190a53314cdfb2162 |
| Source note | uspto-grants-2003_01 |