HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trimethyl orthoformate → 2-(2-(Trifluoromethoxy)-5-(3-(trifluoromethyl)-[1,2,4]triazolo[4,3-a]pyridin-6-yl)phenyl)-1,3,4-oxadiazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trimethyl orthoformate | HCID 9005 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | Ethyl 5-bromo-2-(trifluoromethoxy)benzoate | HCID 44829039 | — |
| Reactant | 3-(Trifluoromethyl)-[1,2,4]triazolo[4,3-a]pyridin-6-ylboronic acid | HCID 58118915 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 2-(2-(Trifluoromethoxy)-5-(3-(trifluoromethyl)-[1,2,4]triazolo[4,3-a]pyridin-6-yl)phenyl)-1,3,4-oxadiazole | HCID 86650230 | — |
Reaction Steps
To a round bottom flask was added ethyl-5-bromo-2-(trifluoromethoxy)benzoate (0.638 mmole) in ethanol (10 mL). To this solution was added 1 mL of hydrazine monohydrate and the resulting mixture was refluxed overnight. The reaction mixture was evaporated in vacuo to give A. To A was added trimethylorthoformate in a heavy wall pressure tube. This resulting mixture was heated at 100 C for 18 hours. The reaction mixture was concentrated down and purified by preparative TLC to afford B which was coupled with 3-(trifluoromethyl)-[1,2,4]triazolo[4,3-a]pyridin-6-ylboronic acid using methods disclosed above to give 2-(2-(trifluoromethoxy)-5-(3-(trifluoromethyl)-[1,2,4]triazolo[4,3-a]pyridin-6-yl)phenyl)-1,3,4-oxadiazole.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08754103B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-2446a601984e40e08b9fc71e2499ceff |
| Source note | uspto-grants-2014_06 |