HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butyl isocyanate → (R)-1-tert-butyl-3-(5-(2-(2,5-difluorophenyl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidin-3-yl)urea
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butyl isocyanate | HCID 62412 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| 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-tert-butyl-3-(5-(2-(2,5-difluorophenyl)pyrrolidin-1-yl)pyrazolo[1,5-a]pyrimidin-3-yl)urea | HCID 46188752 | 82.5% |
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 2-isocyanato-2-methylpropane (9.4 mg, 0.095 mmol) at ambient temperature drop-wise, followed by addition of DIEA (0.028 mL, 0.16 mmol). The reaction was stirred for 4 hours then concentrated, and the residue was directly purified by reverse-phase column chromatography, eluting with 5 to 65% acetonitrile/water to yield the final product as a pale-yellowish solid (27 mg, 82% yield). MS (apci) m/z=415.1 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09127013B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-3cb5c0946b5b45e780e1ef3e4514d56c |
| Source note | uspto-grants-2015_09 |