HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phenyl chloroformate → HCID 59380121, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phenyl chloroformate | HCID 15891 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 59380104 | HCID 59380104 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 59380121 | HCID 59380121 | 99.3% |
Reaction Steps
Phenyl chloroformate (0.413 mL, 3.29 mmol) was added to 4-[4-[2-(3,5-difluorophenyl)sulfonylpropan-2-yl]-6-[(3S)-3-methylmorpholin-4-yl]pyrimidin-2-yl]aniline (1.46 g, 2.99 mmol) and sodium hydrogen carbonate (0.377 g, 4.48 mmol) in dioxane (25 mL). The resulting slurry was stirred at RT for 1 hour. The mixture was partitioned between ethyl acetate and water. The organic solution was dried (MgSO4), filtered, and concentrated under reduced pressure. The residue was chromatographed on silica, eluting with 25%-80% ethyl acetate in isohexane, to give a colourless gum. This material was triturated with diethyl ether to give the desired material as a colourless crystalline solid (1.808 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07750003B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-3fcc8259b2404d789e920ceb07662dcc |
| Source note | uspto-grants-2010_07 |