HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxide (P4O10) → HCID 44595336, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxide (P4O10) | HCID 14812 | — |
| Reactant | Bromodiphenylmethane | HCID 236603 | — |
| Reactant | 5-((trimethylsilyl)ethynyl)pyrimidine-2,4(1H,3H)-dione | HCID 12782037 | — |
| Catalyst | Chlorotrimethylsilane | HCID 6397 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 44595336 | HCID 44595336 | — |
Reaction Steps
2.09 g (10 mmol) 5-TMSU (5-trimethylsilanylethynyluracil) dried over P4O10 are suspended in about 50 mL absolute MeCN, then 6 mL (25 mmol) BSA and a few drops of chlorotrimethylsilane are added via a septum, and the suspension is stirred at room temperature under argon until it is completely clear. Then 2.72 g (11 mmol) 1-bromodiphenylmethane are added to the resulting solution. The batch is now stirred for 24 h on an oil bath under exclusion from moisture at 84° C. The dark brown solution is concentrated and left to stand in the ice bath. The brown raw product that precipitates is separated, washed with a little cold MeCN, and recrystallized from about 50 mL MeCN.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09181199B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-aeb82489c84a44028dd8506fcb8daeba |
| Source note | uspto-grants-2015_11 |