HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 5-(Benzyloxy)-3-bromopicolinonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Trimethylsilyl cyanide | HCID 82115 | — |
| Reactant | 3-(benzyloxy)-5-bromopyridine N-oxide | HCID 58213489 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 5-(Benzyloxy)-3-bromopicolinonitrile | HCID 67117707 | — |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
To a solution of 53-(benzyloxy)-5-bromopyridine 1-oxide (from step 2) (1.0 eq.) in acetonitrile (0.2 M) was added trimethylsilyl cyanide (TMSCN) (4.0 eq.) and triethylamine (3.0 eq.). The reaction was heated at 100° C. overnight. After cooling to room temperature, the solvent was concentrated en vacuo, and the residue was purified by a COMBIFLASH® system (ISCO) using 0-40% ethyl acetate in hexane to give a mixture of two benzoxy regioisomers, one of which was the desired product. The mixture was carried onto the next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08466167B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-9b526edc860d480e999b830be89590ee |
| Source note | uspto-grants-2013_06 |