Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Diethylphosphite | HCID 3780918 | — |
| Reactant | HCID 86588647 | HCID 86588647 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 86588646 | HCID 86588646 | — |
Reaction Steps
To a solution of 5-benzyloxycarboxyamino-1,3-bis(trifluoromethylsulphonyloxy)benzene (5 g, 9.78 mmole) in anhydrous acetonitrile(320 ml) under argon was added diethyl phosphite (5.9 g, 42.7 mmole), triethylamine (5.95 g, 58.9 mmole) and tetrakis(triphenylphosphine)palladium[0] (870 mg, 0.75 mmole) and the stirred mixture was heated to relux. The light yellow solution was refluxed for 3.5 hours then cooled and solvent removed in vacuo. The residue was partitioned between ethyl acetate and water and the organic layer washed with 1M hydrochloric acid, water and saturated sodium bicarbonate solution then dried over magnesium sulphate and evaporated. The residue was crystallised from ethyl acetate/petroleum ether bp 40°-60° C. to give white crystals
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07572459B2 |
|---|
| Source dataset | uspto-grants-2009_08 |
|---|
| ORD ID | ord-e5f60531fd274a34b5c5e97daf9b5611 |
|---|
| Source note | uspto-grants-2009_08 |
|---|