HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phenyl isocyanate → (R)-1-(5-(2-(2,5-difluorophenyl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidin-3-yl)-3-phenylurea
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phenyl isocyanate | HCID 7672 | — |
| Reactant | (R)-5-(2-(2,5-difluorophenyl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidin-3-amine | HCID 58386314 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (R)-1-(5-(2-(2,5-difluorophenyl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidin-3-yl)-3-phenylurea | HCID 46188753 | 87.4% |
Reaction Steps
To a DCM (0.8 mL) solution of (R)-5-(2-(2,5-difluorophenyl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidin-3-amine (Preparation B; 25 mg, 0.079 mmol) was added isocyanatobenzene (19 mg, 0.16 mmol) at ambient temperature drop-wise. The reaction was stirred for 5 minutes then concentrated, and the residue was directly purified by reverse-phase column chromatography, eluting with 5 to 60% acetonitrile/water to yield the final product as a pale-yellowish solid (30 mg, 87% yield). MS (apci) m/z=435.2 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09447104B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-9d001a8435bf425eb3d32ad8b68d1d56 |
| Source note | uspto-grants-2016_09 |