Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Diisopropylamine | HCID 7912 | — |
| Reactant | Tris(2,4,6-tribromophenoxy)dichlorophosphorane | HCID 194959 | — |
| Reactant | HCID 178491473 | HCID 178491473 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 178491472 | HCID 178491472 | — |
Reaction Steps
A 250 mL two necked flask equipped with a magnetic stirrer, a gas inlet for argon, and a septum is assembled under an argon atmosphere. All glassware are dried at 120° C. for 1 hour. The flask is charged with N6-Benzoyl-5′-O-(4,4′dimethoxytrityl)-2′-deoxyadenosine- 3′-O-(2-diphenylmethylsilylethylphosphonate) (0.015 mole) and diisopropylamine (0.12 mole). Anhydrous acetonitrile (200 mL) is added. To this stirred mixture under argon at room temperature is added tris(2,4,6-tribromophenoxy)dichlorophosphorane (0.225 mole). After stirring for three hours, the reaction mixture is filtered, and concentrated under reduced pressure. The crude product is purified by flash chromatography using silica gel to afford the desired product. Triethylamine (1%) is used throughout the purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06441150B1 |
|---|
| Source dataset | uspto-grants-2002_08 |
|---|
| ORD ID | ord-af1a60c5d03e426786a2403991591ff9 |
|---|
| Source note | uspto-grants-2002_08 |
|---|