HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → Benzimidazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | L-Tyrosinamide--hydrogen chloride (1/1) | HCID 45157672 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | Benzimidazole | HCID 5798 | 72% |
Reaction Steps
To a room temperature solution of intermediate 2 in anhydrous dioxane (200 mL) were added triethylamine (6 mL, 40 mmol) and tert-butyldimethylsilyltrifluoro methanesulfonate (8.6 g, 32 mmol). The resulting solution was then stirred overnight and quenched with saturated aqueous sodium bicarbonate solution. It was extracted with dichloromethane (3×100 mL), and the combined organic layers were dried over sodium sulfate and concentrate in vacuo. The residue was purified by flash chromatography (silica gel, hexane/ethyl acetate) to provide intermediate 3 (9.2 g, 72% overall), which was characterized by LC/MS (LRMS (M+H+) m/z: 458.16).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08207340B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-ddd7e7e3207340729a7a5ec54e0fcf0e |
| Source note | uspto-grants-2012_06 |