HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitrogen → HCID 57556918, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | Triacetoxyperiodinane | HCID 159087 | — |
| Reactant | HCID 12001224 | HCID 12001224 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 57556918 | HCID 57556918 | 69.6% |
Reaction Steps
To an ice-cold solution of compound 10a (320 mg, 0.92 mmol) in dry CH2Cl2 (10 mL) in a N2 atmosphere was added Dess-Martin periodinane (DMP) (600 mg) portion wise and the reaction mixture was stirred for 3 hours at RT. The reaction mixture was quenched with solid NaHCO3 at 0° C. The product was extracted with CH2Cl2 (3×30 mL) and the combined organic layers were dried over anhydrous Na2SO4 and evaporated under reduced pressure. The crude product was purified by column chromatography on silica gel using a 3:7 mixture of ethyl acetate and pet-ether as the eluent to afford compound 12a (220 mg) as a gum.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07776900B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-9aa623121a994b5cb649e066de49b454 |
| Source note | uspto-grants-2010_08 |